DISCLAIMER WARNING! This took is intend for informational purposes any! Itis currently egal to atempt almost any procedure depicted in Uhis book. This book does nat condone nor imply that ary proce dure listed herein be used by the reader or anvone else for that matter. Even f the chemist were legal Sirke would not avis derstanding of chemistry. chemical reactions and methodology. Even the most baste chemical or reatton nas the potential tO 00 (teat harm, Copyright ©1999 by Stike, Al ghts reserved. Panda Ink 2211 NW Military Hwy, Ste. 116 PMBY 115 ‘San Antonio, TX 78213 INTRODUCTION ECSTASY & AMPHETAMINES WHERE To BUY. WHAT TO BUY. HOW TO MAKE. METHodology. PRECURSORS PHENYLAGE TONES METHOD #1 METHOD #2 METHOD #, METHOD #5. METHOD #6. METHOD #7 METHOD #8. METHOD #9. AMPHETAMIES & METHAMPHETAMINES FROM PHENYLACETONES. Me IHUU #1 METHOD #9 METHOD #3. Me HOU #3 METHOD 45 METHOD #8. MEIHOD #7 METHON #8 METHOD #9... METHOD #10. J-NITROPROPENES METHOD #1 METHOD #2 ‘on 103 oT) 108 116 MW a7 120 422 1 7 131AMPHETAMINES FROM f-NITROPROPENES.. METHOD #1. METHOD #9 METHOD 43. METHOD #4. METHOD 35, 'BROMOSAFROLE & PHENYLISOPROPYLBROMIDE, ME MUU #1. METHOD #2 METHOD #3. AMPHETAMINES & METHAMPHETAMINES FROM BROMOSAFROLE & PHENYLISOPROPYLBROMIDE METHOD #1. METHOD #2. METHAMPHETAMINES FROM AMPHETAMINES METHOD #1 roo METHOD #2. METHOD 38 ADVANCED SHRIMP PREPARATION TECHNOLOGY RHODIUM'S CHAPTER. PROMISING THEORETICAL METHODS. BUILD FROM SCRATCH. ‘SALICYLALDEHYDE. METHYLENATION. BROMINATION OF 7,3-BENZODOIXOLE. THE BIG CHAPTER. THANK YOU SIR MAY | HAVE ANOTHER? CRYSTALLIZATION, CHEMICALS. REFERENCES, EPILOGUE, 137 138 130 139 140 14 142 46 148 152 152 158 450 159 139 160 161 164 102 205 208 214 222 232 240 47 “252. 285 201 INTRODUCTION ‘You have just purchased or colon the most comprehensive and detaled book on the underground production of ecstasy, metham- Dhetamine and psychedelic ampretamines ever published. Strke {yur host) ian ecstasy and amphetamine chemist fom Texas Who used tobe very ustrated with he lack of common-sense fr this for Strike and now Strike is gonna remedy it for you, too. Tis ‘book is packed with te latest street metrods for making am photamines wien In lain English with the deta that ne athor book can offer Pus ths exlton of Total Synthesis marks the frst ever collabora. ton ofthe chemical underground, Throughout he book you wil leacing underground chemists. They have spares thelr knowedge ‘so tat you may ge te Gest egucaton avaiable So enjoy!WARNING! This book i intended for informational purposes ony! Ikie curry Boga! to atempt almost any prosodure dopited in this book. This Book does nat condone nar imply that any procs. ‘re isted nevein be used Dy te reader or anyone else fo that ‘matter. Even if the chemistry were legal Sirke woul not acvise have a thorough ur- Even the most basic chemical or reacton nas the potential fo do great harm, EUSIASY & AMPHETAMINES The reasons Stike wrote this hosk The raacons youre coading tis book. Ecstasy i the most benign chug Strike has ever en countered. itis passive yet gow By powertl StIKe 0OeS Net ‘mean that it ineapactates or makes one danaerous. Ii in fact {ute tne oppost. is powor Is nis ably to evoke a total sen- sy hath of tact, visual and mantal enhansemort One's per capt is perecty dear. Halucnatons are nonexistent. The foslng vow has 8, Heraly, ecstasy.” PWS, fs one ot te few Nar ates in the world tat i not physically adcetve, Why tis sub. since was taken avay from the people Is a question that only goverment funded eigntate can anew ‘cers nox rxger mam (spee0, crank, cyt), Then again. any ont we just forget about them. Momma sat you cant say ‘anything nice... cis Cosfecsasy class drugs and speed class drugs can De seen in Ine Prscading schematic MOA and ito brother, amphotamine, are the easiest to make, in ‘yolve the least watched chemicals and are the etrngest MDMA ‘nd speed, although less strong and shorter lasing, are perceNed ‘and more pleasant. "This is not necessarily true asthe degrees of “ferences between MDA and MDMA or amphetamine ard speed fare very subjective, They are equally fine in their effect except that MDA Te batter. The sooner the chemist accepts the, the ‘easier her Journey through underground eynthesie wil be in many Fespects. So, wnen Strike uses the blanket term of ecstasy Or X throughout this ooo Strike may be refer Io witier MOA ot MOMA (most MDA), Strke wil let vou kaw when @ speciic ‘fferenca is requred. Anyway, if one were t ook at that nitrogen ‘atom stuck on tre MDA oF amshetamine core one can see that Tore earbon groups are added on, the weaker the drug becomes, SoMDEA and PEA are even weaker tian MLM an speed, out they do retain some pretty fair actly. And a few panes away you are going to actualy Year every excruciating deta of how under- (Found chomists make every sng eno of thee eompour ‘So how does one go about beginning an underground laboratory? ‘The answer a: "they don”. You sae tet would be ileal Hypo™ thetially though, one would need 3 things: a combination heat- Ingsmagnetic sting pate, ‘emicals and. glassware. The problem. But Stike is going o go over how all ofthese things can be sought subetiuted or or made, Good production va be fad with crude, makeshit equipment. But believe Stik, the most fective chemistry possbe le achsoved wih a good heating strplate land's ground gas satiation kt So late see how the good stu Can be had before we discuss the back-up plans. There are bas ‘aly four ype of businesses va Uite Unt ule fo people Heed ina Scientist (1) Lite, local wak-up ype sores ‘These kinds of stores carry haboylat supplies, gimmicky s3- cence far projects, art faims and a tow assorenen of base Scienceware products such as beakers, thermometers, scales, rubber stoppers and most af the basic chemicals such as sede, bases and solvents, These placce are leted inthe chemicals tion of any big city's yelow pages and are relatively safe places to {Get most or ne Das 1aD necessnes. Ne crawoack 1s mat mney {are really expensive and dont sell very large quantities of any Chemical is possible to have these places special order a needed chemical ‘neta controled chemi (2) Local miatemen companies “These platas are also local businesses that can be found in the chemicals coction of any big cls yellow pages except that hese fre licenced dsiibulors for some of the biggest chemical and Sciencoware companies and manufacturers. "Those bg coma- ies would never sella thing to purk Eke you or Stike. Even f a punk 'ke you or Strike was to present a fake business front oreoneting thew would senuiniza It ary elngaly ane wet reine posts ofclentelo et. te. Hsrecdiess to say that this is too much to ask of a etret punk ‘Thal Is ere these Gistnouors can help. They have the license ‘26 authocty to sell anything (Gath chemical and glassware) thet the chemist needs and are not subject to the same policies that {We companies they sll fr employ. This ie out oat as pu ‘sown but these cstbutors are ke cat salsemen. The only Way ther make money is through the commission on alee. This ‘mains that they tend not to cam about whom they sal theee other Cmpanies’ products to. Thay just want to sell suf. A chemist Gals one of Urese eompanies and oiders suming simp tke ttemameter or water ana then pays for promplly” Having then ‘tibished an account (a foot nthe doer) the chemist wil have teited that companys tt in knowing that he (te chomist) fo eat customer. Then, next time, a ite catalyst, ether of per- Siam, a iaiun hk cas bw unieies, raving aesay estapisnes thal the chemist is a good customer thay tend not to ask forthe required permit to buy glassware or as to the purpose that some chomical i needed far And a the charade gove on ‘These typas of businesses are the prime enol a chemist wil use tovset that speciaity chemical or piece of alaseware. Therm arm thossands of euch places around the nation, Canada and Mexico, (@1National ditibutors ‘Tachomist were f2 go down to her local university or graduate restarch schoo! she could find science comaany catalogue in the Tray and in the divisional abs and offeas ofthe research canter Repesentatves of every eancowabio scioncowara company and rmavufacturer Ike to drop off tons oftheir catalogues inthe hope thar sumeone wil order some otter procuets. tte horary has nore. then tha chemist ages un to nn nf tha lane and) ache fsureane it she could take a look at soma of ther catalogues, ‘Ts nota probiom becauee the labs ars full of graduate stor ders who are dying for atenton, Some have £0. many cat Iegue’ they dont use iat, 1 a6Ko5, they WoUlS Probab gwve the ‘chem st some. -10 \What the chemists looking for are product companies that sell everything but glassware ana cnemicale. The reason tor ths that if they know they dont sell anything that is watched thea thay hhave no reason to care who buys their suf. In fact, they want f0 ll tho chemist otf very badly. The other ypes ef eelalogues (0 look for are those that accept credt cards and money orders as payment. Inese companies obviously sell to individuals. All of the chemist needs, especialy low priced magnet siplate, vac- ‘uum pumes,plastoware (great altematives fo some slaseware), flecronic scales and, in some instances, chemicals and alae ware. These companias are jus ke local dstnouters only ger (4) Big name science houses and chemical manufacturers ‘Tee inclule outs names as ener, Baxter, VR, Cole-Parmer, Altech, Akich and Slama I is very hard to get a fledaling 2c Count with these giants butane can than the sky's the limé Most chemists should be happy geting thees companise’ products through the cstbutore [No matter what tyne of company the chemist chooses to purchase from it is a good Idea to have some ofthe actual catalogues from the bg name scones houses and glssouare manufacturers, This Ie because wil holp to have the company's tua’ product cata: rogue numoer wnetner one Ts oreenng tom a cistibutor of om the comsany itself (ocks professional bubbal). These realy big Catalogues are down atthe university or the chemist can request ne from the company isl. They abo make excel reference books and are just plain interesting to read and daydream of he day when one can order suchvand-such an apparatus 28 Is de- peeled on page whatauar Chemist to order. The folowing Is an example of how a typical cll Will proceed and how it wil be handled by @ chemist no matter ‘what melnaes aha elle =Ring!Ring!~"Uh, yes, this is Fake Name calling for Fake Com- pany. Name and I need to order some tems or possi open an ocaunt” FRop. "Does your company curently have an existing account with oer | they anways ask tis wnether or not mney were just tla tnat a ‘customers anew one | [Evil No, wo Ueed to have an account with Rival Selene Com: pny but they couldrit seem to get our orders on time, ‘op: “And whats your company s name and aadrass* [They ask this frst because they want to bag the chemist as cus- fomor ora loact got thom on a maling Fat s0 that ay can hound the chemist later fo buy more ofthe stu] Evi "Fake Company Name, at Address Of Francs Housn* [ Delivery Wo an sparinenl aldose is unwise a tere ae very few companies at wll daliverselence products to a PO. box) Rep 0K Mr Fake Nama, wat can wi da for yu day" Fim tne Svea tales ui te vase ants of te Sigs ‘she wants and the quantity of each. Alter the order is confirmed the chemist asks thatthe entre order be shipped by overnight e rose and has this arfed t th total il ‘The shart then ask {or the purchase order number ofthe purchase she just made $0 {hat she can include this on the payment sis going i send, The ‘chemist uses a reputable money order and sends tis money or- der to the company via pronty overnight mai Allths rushing ac- professional, goal- orented company, andi also gives no one any time to secon gues a thin or etabish # stakgout of te dee ory site ‘cat-and-mouse afar that leaves suspicions high {and faces put or unes pone line. This cannat Be futher fom the truth. These comaanies want to sell ther prodets. If tney hat to flo notice to tre DEA or demand documentation every time someone caled then thay would be broke in'a weak. This dove rot mean that a chemist should be carcass, Its just tat if 2 ist putts, feely ane smare then almost anytng can be had. And Since, 26 this Book wil agit eit mast everthing the Chemist needs wil Be unwatched, thera wail not a great deal of ‘sutpicion no malior what tho chorit ordore. Just remember one thing: the chemist never orders anything to the same place she oaks at Science dealerships arent the only places to get the stuf one needs, At those moga hardware stores one can fin pure aceon, methanol, ethanol, toluene, metry! ethyl ketene, DCMS a con: ‘sttuent of some sinpoing agents), sodum hydroxide inthe form of Ive, and some acide auc a8 stfre and hychochlorie Those. precious tools can be bought there cheaply and in great quant, ‘Then there are other paces such as chemical waste exchanges, pool supply companies, elecroolating companies, photography Sunny shops, agrcitire companies, specially gat conster com panies and just about anyplace where @ chemical can be sold Finally, one simply cannot find the thing one needs then t's time to hi the bibes of ndustial and commercial sources! “Chemical Fuyers Wao’, "Chamenuree USA." and the massive "Thomas Registe”. These thee source books can be found at most lar fs aod contain the Iisings and services of just about every Bus ‘ess inthe country. No matter whal the chemist needs, it can be found in these books. Even it takes going oneby-one trough ‘she needs and someone that wil sel it io her. ‘The one source Stike dows not condone is theft. Ifyou steal then you are a weasel anda cowardGLASSWARE ‘saty, me cnemist wants @ cstitavon kt wan jones mat are of ne ‘Sze 244b{d0 ek) Thi th most vergatdn int san for ar ‘Commodating etn large and small asks." Speaking of flasks, the ‘ype one wants these days ere flat botlomed flasks, not ound Dettomed flasks. Flt-bottomed flasks allow one to heat on flat Surfaces such as a heating str plate. In the frst of many beautiful, hhanduaaun skatchas thal wil appar theughout thi fae book ‘one can see the components and proper configuration ofa regular ‘tiation eet up in toue 1. Olher paces of glasewere Wiel ae highly desirable but canbe led without or made (as shown later) fre shown in figure 2. ss Co) CeeN (Fioue 1) oe Now naw ie ang ta eee mae hase ema a tng er rescore, savers, acde and bes fo bo ha Cerosieat) type aieanware Boe Abrode ana exposed to aise marth Choro fied condone Thane itnger toe Any reacton | Pyrex anything ese wl met OF ‘adn inn in is Book that does not re- ue direct heating can Be dona in a polyropyt- tne (PP) or povethyiene (PE) conainen, Tis fs sapntareny Tegardiess of the chami- ease Cals eves, Pobpro: “Sok iene (8) ang payethylene (PE) ate Ny Sop nen ara fericey restart (0 amet an ‘Sg ts book describes Susie, abn hon, Sandal sor of conten mee ara ‘ants, opeae, nee Blable slate. can oe Powe 2 found for pennies at any dicount or grocery store, Those con- homta fru in lassvare. As was mondoned car late ware Sarin to mane to anc n baogeal and Som abe Bucher final, side am fasts, ast yan at mer feparatoy funnes come PE and Pe, Thowe gusoware eb S%e3 aro he bootie choos fortedays com a hey aro oe watched, versatie ard 110 the conto gles the creme Sse wat pasta containers hens can lok fore oe Son be anaeanen comes vacuum ‘The cheinists going to need @ source of vacuum. When distling righ Doung stu Ike Valuable ecstasy free base ol, a vacuum 1spressure insio Below the normal siospneric pressure outsie. This causes ever Fthina to Bol ata much lower temperature. I high boling ols are Slowed fo distill at hei normal temperatures and atmospheric prosture thon 2 canaidrable amount of prot cn lot in {o scorching, The other purpose fora vacuum is for vacuum fir ‘on, whit sa very use process ais Uesctived lar on ‘Aay commercialy avaliable vacuum pump s perfect fine forthe Underground chemists neads; but tha bee! Kind to buy ie 8 lax Bhragm pump, which s more resstant to the often-harsh chemical apors that are sucked through f.Most vacuum pumps cost about '$100-8200, However. the stonaer the vacuum the beter. if a heist acing ul rm of He (Get ah ke begs inthe Shemisty papors do thon he san be leaking at a turbova. can run wal over $5000, ‘The other vacuum option is a simple litle aspirator that attaches to cones faucet or hose. Ths 815 device ouls @ decent vacuum; However iis nolan option at ain Stike’ book, Running one of those babes 10-12 Ws @ day is @ despicable waste of a commu rity’s water supply WATER PUMP ‘This i going to supoly the cold water that courses through the condenser whether thal condenser is Setup for reflux ors part of 2 datilaion corfguration. ‘The pump nood nat bo vory atrong. In fact, the perfect example is one of those ite, submergile fish tank pumps that ane can nd at any pet store for about $10. All the chemist dons i atlach @ hose fo the outiet. chunks the ile pump Into @ bucket of ice water, attaches the hose to the con- in junk yard. The chemist removes the reservor (pump st at {tached}, apniies an avant power source to the pump and USES the plastic servo fo Rol the ice water. HEATING AND STIRRING ‘There relly io no gacd eubettte for a combination hosting and magnetic stirng pate, noc is there any reasonable excuse not to {get one. These are perfect legal to buy and can be founs st any ‘Science outlet for about 200-400 dollars. Here's ane area that te a surface area as possible is a defnte pus Late jut suppose, hypothetical thatthe underground chemist ie 100 stupid or unwiling to get a sti plats. inthis case a single unt pottabe hotplate can work. bul contolied heal using ese f best Accomplished by water or oll baths. Sting can be accomolished byallacning a shat and paddle to 8 power dil or any ger drivenStrke Is sure that an imaginatve person can look around her eve- ryday surroundings and think of fomathing that can act @ =~ Placement for seme of those hard to get glassware Rema and ‘ther gizmos. As itso happens Sirks has thought about this too. made, (Fas) ois ‘The best replacement fr borosilicate glassware i eainleas stot Stainless etaol takes te heat, wort brook, ond, moot Importanty, is about as resistant to chemical degradation as the chemist can ope to tnd. For mose tems mat wont De suOjaced {0 dtect heat there can be some steelimetal or steapastc hybrids In g- lure 3 is shown how flasks of any size can be made With two ‘anise otcel mixing bows weldod together. Als slur fs Ue vacuum adaptor and condenser. For the condenser only tne ier ibe need be steetThe outsde pips can be coppe: or something [As for tha ather components of eatitation setup. well hey are made just as they look In figure 4 is shown how @ separatory funnel and a pressure ‘equalized adation unre! are made. The funnel part ie just @ PP fre! from the grocer less stoe! ball vave, See how the addon funnel is made by us Sig 1oouer stopper ang am oxta extension er tong Tome tp the funnel? We, thats how ene can make a sealed addon fare el out of the ordinary glass separatory fuanel that one gets nth a elation Kt ar rom wmorever, = xe ( SX / h) an o i (Fe »All of the nieces pictured here are not going to 6 pncarty inn teach othor and that's going to causa all sors of leaks, The an- ‘Wer ia teflon tape. Stike loves folon tape! Ths Inexpensive Product Ig found in the plumbing department of any harsware Sore and is the duct tape of the next cenury. Tefon tape is Chemically and thermally indestnctiie ‘Thie stff is wrapped ‘around any piece of pipe oF jor, said part then jammed in te appropiate ‘eveptacie and the pe wil oid lo fo perfect Hell it can mummy @ whole joint complex to make it absolutely impregnable. ‘So whats the downside of using a slain steel ditation kit? ‘Tie chemist cant see shit! There isa define aavartage of Deng able fo see a reaction as It taker place and to eee when some thing starts to cstil over. All Strke can say is that the chemist ‘must rly mush mere heavily on tre readings of her thormometer ‘and have @ greater faith in the chemistry she ts doing. By ths Ske means tnat since there ie probably gomng to be no more than 2-3 different chemicals in the reaction flask, then chemist need be aware of is what thing comes over frst, second snd last. Stiko knows. Dike hows. Hf a ibe more compen than that, Buta chemist gts the hang of ditilation realy can De as simple as that PIPE BOMBS, ‘Abie bomb is not a bomb. Is just a device to hold high boiling or high-pressure reactions in an enclosed cell. The bomb should be Inade fiom a seins steel pipe at sa big oC a inner aeme= ters possible (width, bubba!) There are to good configurations which can be seen in figure §. One end is permanently sealed by Welding, The othe end, miter which contyuration is used, Should have as much and as fine a threading as possible, Also ‘when sealing up the pipe bomb, iti 2 great idea to wrap a lot of teflon tape around the tueads then sciew on the esp. This will form an absolutly air tight seal. It is also possible to substitute a Salnless see presure cooker for some sealed, pressured restion, -20 GIRLS IN DA HOOD Some ofthe reactions thatthe chemist may use wil just naturally sme bac. Usually somerning smels bad then Ws probaly bad for the chemist to smell i Some reactions ave. by desian. sup- posed to vert bad tings thst, when unchanreled, have nowhere no guarantee that a method wil go as planned. There may be @ Mistake or unforseen side reaction and some of the most deadly shitimaginable can be evolved. That is why the chemist wil con- Struct the one thing that may end up saving her Ife: fume hood, omeIn professional laboratories fume hoods are bia metal boxes rest: Ing on countertops and are connectes by dus to biower mators fon the root ef the acity. Tha blower mator is conetanty sucking the air rom the hoods fo the outside so that chemists wi not be exposed Io he vapors of ehemicas they are working Win side tha hood. The Same precautions are taken by non-dead under: (round chemists (Fig) 7 ‘A fume hood is constructed in the manner shown in figure 6 ‘Srke deo the fame ao being made of lumber but can Be made of rebar e*, preferably, rom PVG pipes and joints so that t can be assembled and disassembled with ease. The frame i. enclosed wih plastic op cathe oe ary namilnar paste shosting, Tho front face of the hood is halfway covered with plastic while the boll half is exposed io alow oe to move objects of out and to manipulate things. On toa of the chamber is attached cma clothes dryer ductor some such erap which ied to 2 leaf bower fr hlower motor. The exhaust from the blower i led ay to the outside. ‘Although @ lea biower is probably way too strong it may sill be adequate at its lowest setting, To Insure tat @ corectaifiw is boing plod the chamist elds a it cigarete about a foot fan of the hoods opering and looks to soe i the smoke tal le being putea into ie nooa. so, then the nod Works jut fne Many houses have outside-venting blowers over thelr stoves, Gromists in those sual ‘ver, chomisis who Ive in apartments never ever attempt any Chemistry at alin thee paris Why? Well, na! any a apartment stoves lack an outside vont, but to vent a constucted hood Enuuyiva viicy ot uui winiom wi Su seisy Gowe reeghoors living about is ue! plain stupi. 18 also stupid in anather very Important way. lf & chemist fucks up and blows herealf up oF stare fra then she fa not only harming harse! bet le alze going to put alot of her neighbors auton the soe, inthe hosptal or in le morgue. No ome making dus has the right to jeopardize ct fers inthis manner. Thats why drug making is aways done in a house, bam, mobile home (watch out for tornados), submarine oF 2Justin case you are not familar with basic laboratory procedures, {hia chopte wil explain them to you. These are the most base Ia techniques and almost every method in thi entre beok wil = {ure many, t!nct a, f the protecos te flow. So pay attention! DISTILLATION You see that clsilation satup in fg. 17 Wall, when ana puts something into the reaction flask and heats it, low boiing stuf ke frganie solvents (acctone, ether, DCM etc} vaperize and then condense inside the condenser. They then dip down Into the re- ening Task. Next (usually) comes water, then tinal (a far 38 tig chemistry is eoncamath came High ring Amey ce et lation isthe moet preferred and relate way to purty substances from ene anether. ‘There are three basic forms of dstilaton: simple, vacuum and {racional dition, whien ean he an extension of the fat t, ‘Simple stilaton is just pain old dstilaton with no vacuum and is ved for puriicalin of low boling mises of Tor renovig solves ‘such as ether For vacuum csllaton a thick walled or renforoed hose is connected from a vacuum pura tothe nipple (lee Ree!) of the vacuum adaptor Appeaton 6 a acim greatly reduces te temperature of boling and is a must for most ef the dilation in Us book. Facional Ustiaion Is merely vac tilatvn ex ‘cept an added glassware component such as a small Vigreux col- tien 6” a Clasen adaptor packed with shards of glace fs placed henwnen the reartian fask and the Sway jain of 2 normal =atup. Either of these addons ereate a gaurilet of extra surface area ‘siete rat ing igus must pass trough I OFOEE TO Core Sense, This affores a greator degree o! separation between ‘mixes of ols that have similar boling points. However, has been Stree ohseratnn that moet of the ule separation in ths boo! ‘sing dstilation can be achieved with regular old vacuum ea: -04- IF the chemist has done the appropriate thing and bought a heat- Ing stplate then a magnetc star ie alvays ering nt the reac. tion ask Ifthe chemist any has a htplate ther the. chert fe going to have to add some boiing stores to the fask. Boling Stones can be sither litle chips of eon, ile waded up balls ot teflon tape cr tle pieces of a shattered porcelain countertop tie. [Al of these things have los of microscopic pockets of this book, especialy organic solvent solutions, need these bolng stones in hen they te going to be heated. If there are no BOI: ing stones, then a phenomenon called superteating may occur whereby the solution wil start to get otter than fs actual toting Point temperature. Evertualy it wit burt ite boing but alot of t wil nave gone sploosh! inte the condense. Not good. ‘Another thina or two to remember when dstiing Is iran alm num fol around the reaction Flask This wil help step heat les 80 that things wil distil quickor and at loner temperature, Gome- times, if one 's going to distil a solution tha fs Just solvent and produc, al nat pure solvent nat comes over frst i pertecly re Usable and shoul be saved fr future extractions. Tho lat thing about dstitation that needs mening isthe swap ping out of colecton flasks. When ating under vacizm i il ‘be necessary 10 remove ie ask tna has colected all the slvent ‘or crap and replace it with @ dean one to enact al the proiit {hat wil be coming over shortly. This swapping of flasks neods to be dene quichy as soon as ihe vacaun hese Is disconnected. By {uick Strke dees not mean lightning fas. Just quick enough £6 {at the hot solution inthe reaction flask does nt get too much hotter ftom the haat scien tis ting on, eemice ft des, ant the vacuum is repped, it may pula Ite form ofthat euperteat REFLUXING Refuxing is allover this book and the proper apparatus to use fs Pictured in igure 7a. The most gerera ting thal wan be sald 225{condenser attached to the flack so that nothing escapes, The Condenser must be suppbed with really cold water, especially whan rafing high baling lutions f Fava) (a 0) You 200 that vacuum adaptor stuck to tho top of tho sandonaor in fig. 7a? Wel a closer look a it in fig. 7b wil show that it has ‘some arying agent sanawicred between tWo Coton balls ang ine nipple (tae hee) sealed with olastic wrap or fl. The cryin agent {an be efter a commercial produc called Drierite or calcium chlo- fide. Ths attachment ie placed on top of a condoneer whon ro. ‘uxing solutions that nave no water in them and must remain that ‘way during the time hey are refluxed. Al ns isto prevent mots- {ur Inthe outside air from coming ino contact withthe cold sur- ‘ace ofthe of the inside walls ofthe condenser. This wil surely happen ar the condensed oulsiverat water Wi dip don into the reacton flask and uin the experiment. This is not so much a 226 concern when refusing large aqueous solutions such as acid or base hydrolysis seen later n this book (One side note about the drying atacrment i that need not be @ ‘vacuum adapter. Anything, such as afunnol, that can hala a plug of crying material and ft saugly ro the candenser wil Work, EXTRACTION In this book extraction is anos abvays about using an oeganie Solvent uch os berzano, DOM, eth ether aia ether) and hex: Sno to remove (oxtou) roduc fatal stays ro fa) ft an aqueous solsion The most baste way fo erat sto pour he ‘aor soon vo a PP canner, add some soWent and str the tani fat an peter afew mintes. Most aqdpoed lab ues ‘large separatory fuel shako the two fauds. When using 2 the stoppers smacked io tho top. Ths fs done by mediately inverting the funnel so that the stopcock end fe facing upward, Spaning the stopsack ta release tho pressure thon eel te Slopeodk The sep funnels gven a guick shake ten vend “jn Tis repeated a euple re nes alr which the pres Sure eroduction wil have prety meh ceased. ‘Tha rll fo then Shake 3 mints an alow their o separate fo 10m aways on top of water ad DCM and hexane are always on the sean Most sclence papers call for things to be extracted 3 times (2X) with ealvont Ske fool thot tha overland thot ono or two. times is usually sufcient. Sometimes one has eo much product fl that toms ts own neavy ayer (usualy atthe batom), nee Is no need extract such a larae amount wih antes In such a cease one woud meraly cain the of from the water or, using a BP container, deca tho water fom the cil The water sol an then be extracted ones wih solvent and the solvent added to the ot oeWASHING Washing Is almost always the act of taking an organic solvent layer (mos kely the one that was obtained from the extraction of some previous aqueous soldon) which usualy contains product Di and mixing (umahing) # uth clean unter then discarding the ‘water. & solvent layers often washed with a diute acd or base sll solution to neutaize anything the soivent may have abseibed from orevious extractions. These salt soon washings ae then followed by clean water washings. ‘Since were on the subject of clean water, tis s as good a tie as ‘any fo ciscuse wat Rind of water i ed ial Us chemi. By Clean water Sirke means dstiled water (JH,O). Al reactions are {o-use astiled water (34,0) only. Al solutions and ditions are to bermade with dhz0 ao welt” Dstilod water alle for abaut $¢ 2 aallon dovm at the supermarket. Tap water is an absolute no-no In chemistry excep for deaning the alassware. DRYING lust as it ia with urd. drying often follows washing and is used {ori the solvent of any water that t absorbed, Al solvents ab- sorb sure waletallhough you cat see fits a good idea tod the solventproduect of ary water, especal before ditilaton, be- cause fs one less thing fo worry about and Because tnere is an ‘f-chans that water may form m aight amount of byproduct When heated with product ol! under dstilation conditions. All one has o do to dry something sto tako a shoot of fiter paper br paper fowl fold to a cane and place lint a furne! About 2 shot glans fl of endo etfat (NagSO)) or magnesium sulfate is dumped inta the fiter and the solvent poured through II ie {so a oud idea ty foivw up by rising the FapS04 wilt a fe fra, clean solvent to insure that everthing gets washed out of the diving agent. The Na;SO, Isa white crystaline salt that tastes le thle sah Ie bind water molecu witha fancy ciesoving fang leaves the solvent water free. Tie way of dying is aso an Option for making some solvers and pure hauls sdoydrous (war Re {er tree, ousbat) tor some of the reapes inthe book that call for such things. Diyng sit absolutely novessany, but iL is a good bet tht i ree Ipe stresses its use then an ev Underground chemist wl doo, VACUUM FILTRATION tnisproceoure 6 used to separate crystanzea product om sok vent 9 fo remove crap and soles from a ould Figure 8 shows the proper apparatus to use, The collecting flask is called aside {am ask and fo that oxtondod ripple (toe hee) i atached a vac ‘Gum source, The thing that is shoved trough the rubber stopper Is called @ Buchner funnel and is usualy made of white porcelan te praferahy. PP. Tha Buchner funnal, when vawed from abn, Gan be sa0n io have lots of pin holes inthe bottom surface of ls Tite paper or paper towel To filer & soliton one atfsches vacuum and pours the solution into the Buchner fur- hel, ‘AI the solution wi go whoosh sta the flask leavina what is calle a iter cake inthe funnel. The liquid that has collected inthe ‘iter cake is then washed with a litle bit oF ve lean wnat ever-kind-of-solvent-) 4) First wash with a volume of Glacial Acetic Acid equal tothe amount of Seazatras Oy boing pracosaod. This wil romove Cugo 10, Pinene end Camphor trom ine oi 2) Wash with weter to remove any sats made from other contami hhanis and to crash out ary partaly issoWved Sarre (ft might ‘emulsify from the shaking, #80, add commen tae sl ts halp i orash) 3) Wash with rectified spirts (ezeotrope of Ethanol + water, also Jsonn as ‘gram sleohor) 9 diasowe tho Sato, toavin the helandrene behind. Of course, ane should use only the amount fr alconar necessary 10 assa¥ve the expected yet of Satta. 1.4 ‘seems fo work, but could be an excessive amount. 4) Setup for sine dstitation. on the water bath, ori you dont ‘wish to recover the alcohol (shame cn you) just heat gory wih 2 -36- sioubc den seiup (wspecany since tis wil toke quite © while ‘depending on how much you have a istivevapareta) 5) Aftordistitaion torminates (Ethanel bots at 7840). tos! your Saale using the physica properties data balow to cont panty, Thacreialy, your product should bo bottor than 89% pure how ‘The entry fr Sarco in Lange's indicates the fatowing popertios ‘Sarole 3 4-methylenedioxyalylbenzene - Bilstein ret # XD-39 Molecuter Weight 162.19 ‘pecme Gravy: 1.70040206 Mottng Point 190 Boiling Point 233-2960 Insolubi in weter, Soluble in Ethanok Miseible with Ether and CCaorerarm ‘Note tat this procedure has been modified fram the eater ver Sinn in that we no lngor itil off tho Phellondrane, rather, wo target i's insolubity in ethanol as a means to separate irom So ‘role, think we cara agree tat is Is@ much Betar way, an? ‘his procedure, Stiko boloves. was not tid by Fleusis Put hie {heory'on the use of partal solbity Ts very old and founded. ‘Tatar, 98 we all aro, by Elousie' unique genius, ow beloved Bee “TDK contracted a Phlippine resaarch laboratory 10. apoly this proposal Hove i what iby sate Posted by TOK on Dacember 28, 1997 et U1:28:34: ‘Sasse/tas OV separationpunncaton This was prety simple and is wel suited for someone without any stein equtpment! ‘Staving weigh. 112 grams sassatres oF Proced 454 grams of 28% acotle acd In 2 Wer separatory funnel. <37e{form its own top leyer. There was n0 separation using 89.5% ‘acete aci. ‘Added 112 grams sassafras oll, Shake for @ couple of minutos. ‘You got an crangish emulsion. Clears within 15 minutos forming two layers, bottom fayer oil top layer acetic acid, eugenol + the Diner solutes. Separated ine oY from Me omers, washed tne dt aver 2 wih fresh JH.O. Weiaht after ace acid & water washes 108.8 (10.8 grams) ‘Added 100 grams denatured alcohol, no layer formed as the oiy product iz mizcitlo in cthancl. Added 20 game of dH,0. Ths Dbuled the ethane! and other product into the top layer. bottom layer containng somo cinanol and safle. Separated layers, placed the ail hata Inyarinia attr breaker Took he Tom Fight 9 238°C. The ethanol and wator come off <=400 ©... The tained @ 238 C. Product was yellow orange in color, suitable for ‘unatover purpose one has in rand! BTW, afer the safle cooled, ‘ha shocked I wath a 24 NAOH soliton fo sea f ary eugene! wes [aft behind, no partioat formed. Bewutiul, TOK! Beaulful Sirke suspects we wil be Seeing more from this ated chemist later onin the book ISOSAFROLE [At this point the chomist has what can ne loosely considered as pute safole. She can use tis for some methods or can convert it fo isosatole for others. Isosafole isthe runner-up precursor for taking %. cannot be found in nature bu var is ede ot a most exclusively stole, I~? Srike had previously writen tat about” the best reope for making isosaffole OX AA tras fo bong sale wit concen) ated KOH (Patassiam Hysrone) In {AN fthanol. This was actualy: the only -38- [208 Stk kw a a hn tn hare ae manors Se ‘ences for in the erature anda couple of vary conan esate pes in the lanamark book “PURALS by Alcaneee ok ae Shuigin. Pioneers in the research of amohetarines fay re Sounds good erougn tor Ske so Someone ser thay Ste ‘gave Ra few shoe, \nat nappens when isomerization is performed is that the double bond of the alhenvane caine migrace ake nae esate call favorable postion between the alpna and beta carsone of he Propy side chain, Thus isosafule, a propenyaenzene, i Dorn ‘To somerize safrala to isosaale one would lk to have pure sae {tole to stan with, This, usualy, Is nt the ease. Quas-pure safole from sassafiae oll 's ok. Svalghcup Sassats Ol 1 probably ok toa, though not recommended, The saa ethan afin Caries Under @ condenser) in a saturated KOHVethano| solution for about 48 day and that's it The tomporaturo of rofux about 120-140°C, ‘owing tothe fact that the ethanol (usually Boiling around 65-70°C) |s salunated wilh the aide sat Now, the ethanol used ie almact alvays anydious, meaning i has no water. The closest one can got commercial to anhydrous sinanui fe Everoear wnicn is vote ethanal and 5 water (130) Pr00f. A lat oF chemical supply stores will nat namry 100% (200 Proof) ethanol because itis a potable (drinkable) product ‘This means that they would have to got a iquot kere or some ofhet state perm to sell the stuf! and that's @ hassle that many dont ‘want to batner wih ‘he producer decided to stop at, mind you, It s0 hagpens that 954% ethanol and 51% water a constant baling mix that no more ethe Nol canbe our fram. That 524 watnr thors to stay! Thees are ‘Ways to remove that water such as producing a temary azeotrope by the adaion of bonzone, but they are hind ofa asele ard ay »not be necessary. Why? Because an alternate reaction for iso- Imerzation would be to use a saturated aquoous water, Zak) KOH Soition inetead of aa senha qn This wil fine the tempera. {ure of refux fo over 200°C but isnot too bad an can be used f Sesived Go, His oh to fomielze in pare wale, Ure the ile i of water (say 5%) In Everclear shoulant effect things too greatly excep ais the refx tomporatue a tad ‘ya are some oF ine aiecrives fr is prone? ei ane ean Use NaOH (Wy) in place of KOH but the yelds wil go down. ‘Also, what about using denatured alcohol instead of pure ethanoi? ‘Bonaturad aloshal is sthanal aartaminated with 5408 methana| ‘The methanol is there because ils poisonous and prevents peo- ple rom using tne ethanol fr erring, Tis mars that places ike the giant hardware stores can carry aalons of cheap contam- ‘ated ethanol as many of you have discovered. This product CAN ‘So now that we have al the reagents out of the way let's see how the reacton proceeds. Inere's the clear yelow “sate” sting in the batter # the flask and the lear saturated KOH solution is dumped in. The solution is heated to reflux etc. and yes, some Crown bypraducte and destruction artaete wil appear. Capocialy ifthe satol Is not pure. These byproducts should be expected to ‘some extent because concenraiee basic (UH) soutons. san be fs nasly as concentrated antic solutors. One is mindful that KOH is fess intrusive towards the delicate methylenediony ring ‘shuctue of fe saioerisusaole molecule ‘After 12-24 hours of refx the reaction i, forthe most pat, com= plete. The reaction mix wil be a dark brown. So what daes one do ary, The solution should be uniformly dark. i any solids can be seen iCmoans thal they are insoluble In ethanol and can be rem moved from soliton by gravity o¢ vacuum filtration through a cof- {ee iter or some paper towels. fi takes a day to dip through the fiter than so-be- Tan ethan! with payload of Isatole wll -40- i ue dark voyndicss ani wasn ts ehanor wan water at tis Point cannat be done because watar fs intly soluble in ethanol (and visa versa) so two layers wi not frm, Fitered or not, the sthanolicosatatl(cometimes jun) I relieved ofits etnanol by openly boing iton the stove or by ditiation. Any ‘ebianol removed by stato 1s saves because Its can and Derfecti reusable (remember it wil sill hava that 5% wee Ce Should not remove al of tho solvent tis way because things can get really hot aly fact as tho lat ofthe ethanol balls away. Most likely one wll and up with a dack ely layer atthe btm of the flask whichis perfety normal. Any solvert that remains wil, bbe noglyiie Because in Ue nex! slop Une cemst fe going TO overwhelm t by adding a butoad of water If there fs about 100- {200m of dare oly layer then a iter or more of water ie pared In anid mixed rely weil. After things sate ane wil 200 a roa litle layer of clear isosatoie form a the Dotto, a murky brown ‘yikes! jttulsion layor in Ue mide and batcish water layer of tp. “The ol separated and the emulsion is deal within any way that is best fom the below mentioned strategies for emulsion fighting. “This parizular amulsion eof very fie partoulatos aed hae ot of Isosaffole int tone i pallet then ane can add solvent (DOM is {yooa) 0 we remaining waterfemussin layer, shake then Vacuum fier The crud remaining inthe fitr is the junk that was causing al the rouble. With it gone one can now extract the remaining Water layer 2 couple mare times with salient ad tho solvent ‘2 the Isosatole ol then remove the solvent by baling or dition to get pure isosatate (70-40% tans, 20-30% o) caused by introducing the water i o slowly acy the water layer wih HCL AS the water layer aces ane wil sze the emulsion Varish. As this acnurs the water layne wil Eghtan a pactiolatas ‘ad stuff stat to ext the water layer and go into the DCM layer. Works every tne. ale{one ie ett having troubi then there i the ol alsfe: ust tow the whole mess info a dstilation setup and fractionally stl. Sok vent comes. trst, water second and (eventualy) isosatole will come 28 wel ‘Sound easy? Wel procedural It's. But the yield can really suck been pleased with it. Sinke wasnt. But what can you do? Wal, someone named Osmium sent Strke a joural reference about doing the exact procedure above Bur carrying lout in a me Z Hot S EUGENOL: tn very large amounts n bay, cinnamon, etove and pimanto oi. goealy smut ban wap Aaa een Lots of trace amounts in many other oils, ‘oP hd mA [ Psy METHYLCHAVICOL: Up to 804% in most basi, cher and fennel 8 In small amounts in star anise and. wormwood <4"Oh. VSN [METHYLEUGENOL: Up to 60% in various parts ofthe basil plant ‘ound 45% in sgherool ov decent amounts 9 ealamas, case Si, mytle, pimento,pistacia, steonia and some forms of tara: ae CH, neo. 1 4 SS [MYRISTICIN: In moderate amounts In dil, carot, celery, fennel, ‘mace and nutmeg (n0 more than 10% tops). Makes Up about 40% Df tha il oF pater anc ean reach po 50.60% of the oF parsley leaves and seeds. Give nutmeg a rest folks! it jst dont have t when compared to parsley and pars. me ©. OSMORHIZOLE: Makes up 25% of the essential ol of chen ‘very nar ns ths hough Ce ALAS a. PHENYLACETIC ACID: Vary important ragrance chemical recently was it banned by the DEA. Fragrance companies s ant baleve they cannot Spenly sell it It makes up 19% of ase mine ol (very expensive) a Ne COOH 2,3,45-TETRAMETHOXYALLYLBENZENE: In varying amounts income parcley ols (hel, just throw parsey olin pot IO gel 8 ‘arab bag of psychedelic amphetamines) H.co. KZ neo SS bor \VANILLIN: In vanilla beans of course, But never more than 2% “This sis bought as a eymtic and ie ches ane legal, ‘You can see from above that some ofthe more desirable alfben- zenes co rot occur m high concentrations in the ots they are {ound in. So that means there Is lt ef eran tne has to etd of to isolate the goods. This is not as big af a concer as one might think eEssential ols trom plants are technically known as ‘volatile’ oils ‘This means, amang other thogs, that Mosk every component of them wil eventualy evaporate if ft to stand, So there i a definite boling range for these ois which, compared to other things in na- fre, ie relatively low. Stee meane to aay that wan these cle ‘were extracied from the plants they come from, they were taken Dy Steam astulaion wrvece steam was te carrie. This eaves you ‘with eomaounds that have relatively iow bola points with 300°C. being close fo the max And Strike can tll You right Now that in ile thal cary allylbenzenes, those same slllbenzanes are alm: ‘always going fo be the highest boling compounds. Usual the Du of the ou consti.tes un compounds thet Bou Well OW the alibenzenes, People with or without cstilaton apparatuses can take advantage ofthis fact. Just Bor dtl off most o the of Up fo the tempera: {ce of Your preteres ayioenzene anc stop, Inere Isa very good cance that what I eft willbe a majority of what is wanted ‘The above suggestion is, of course, cather broad. Most people ‘woud prefer'@ more spectic soluton Unforunately Strike has ne. For over hala year preceding this second eaiton Strke was Patiring money ant tina ini the razatinn of making an iaapenny! Ileredate Gut of soot us sufute act (pease dot 28h) Wil. things didnt workout forthe soprop! intermediate, but dd Confirm the folowing procedure as a nity way of isolating aly benzene (i af} eremicliy “The Iterature states that one uses ice cold, concentrated suture ‘acd on a terminal akene (aka alibenzene) an alcohol (OH) intermediate wil form ‘Markovnikovy’on the secondary carbon ‘has some elem ol and wants that elemien tat i mit What one {ct dof chi, sa, 500nnL ofthe ola feezing and do the same {or about 100-200mLs of concentrated suturcacid (atleast 90% cone) Next, one Just mes the two together for about 8 min. ‘Wat wil happen if that the old He SO, wil mae a hydrogen “0 sulfate intermediate withthe elemicin causina it to miarate aut of {he ol layer and go into the sufurc acid layer And since elemicin |= going tne aut the saly thing in elm ol that nae 2 terminal ‘akene tis going tobe about the only thing that goes Int the acid layer. Presto! Akeve solsted. viel, almost. What tne chemist oes next is separate the acid layer (sil eoid mind yout. pace it in some vessel and pour n a big od excess of water. The tem- perature wil go up and the hydrogen sulfate wi be inatnthy hy {tolyzed by the water to form an OH. One can also heat for 5 What happens during hyccolysis is that the OH forms and the ‘clemicin propy alcoho! dope out of 2aluton and forms ts oun layer Of course one wont see this because the souton ls a big ‘ld brown mess, lousy win emulsion parties. Emulsions suck! But can be deat wih efectvaly by acing litle acc or hase. 07 fiaton and tne ike. Anyway after a tle wock up one gets some Strike would have that OH siuck right on the mide (beta) carbon othe species. Work could then progress on Using that GH to get fn amphetamine (Soh! Srke hat so mich aoc! tat subject thst Strike was prepared 0 put inthis book). But that isnot the case. What the Korean lab found out was that when this procedure is performed, the OH stabllzes on the alnha ‘any use for a is then that is fine But what te most preferable ie {o feduce the OH to get the propeny/benaere (say soelemicn for ‘our example). Using the smple potassium bsufate reduction Fecipe, one can get rid ofthe CH with no problems tal Hey! That realy wasn't a lt of work. Just a fot of tak on Stike's Dall. All oe did was mee Ol with Some seid aed water an 'olated. One gets some oure propervibenzene without distlation, BBone'on a massive scale, tis sa cheap malhod for geting ls of mai cancerteaion alylbenzane. compounds ut of complex 3! mixes. And since Stike blew so much dough oa this glorified ex- Uiaclns protoca, someone better damn wel use a! (In at 2c ‘demi ab ofcourse).‘A much more forgiving yet limited extraction method can be used to tolate phenol Species such as eugjenol and chavcal. You see factner back i this chapter where one an use diute NaOH to re- ‘move eugenol fom sassafras of? Well why not use Kt to lalate the damn things for further research works fea charm! Tere are prebanly otner methods for purtying the products one eal sense ofthe word. Strike has no rea dea ofthe tue applica. tion of chemistry and takes a ot of guesses (why is Sith teing you tis?) But on the Hive, Strke gave ita few stabs. Things Ike Fecrystalization (don't ask), paral soluble lke what our fiend louie propated abou, reazing, heating, fiezing-and-hecting in 2 wo solvent system, sald phase extracton and aerate fo7ms ot camo pulicalion. Or owe can uve any of Ue above fn ont bination, All ofthese are ways, that an industrious chemist may ‘wish fo futher study and apply. So ht the lary, Bat ‘And now forthe hardcore chemisty youve been waiting for. PHENYLACETONES So let's say, for instance, that some deranged lunatic dd the exact ‘opposite of what ths Bock says, and weat ahead and got some eatipment, 2 couple of chemicals and some saicie, ovale “andlor the precursor of thet choice. They may very wel deode to 4o sometning toi to gett father along the path to fal produc, Wel curently on the place calad Farth, the most widely made Drecursor for X and amphetamine production isthe phenylace: {oye, For cysial meth the precusor iy caled just that phen ylacetone (aka. pheny-2-propanone, aka. P2P). For X the Drecursor would ‘be caled 3 4telhylenedionyphenyiacetone (ka AAMethylenediony-shenyt2-ropanane, olen. MDP2P), Strike knows it should technically be witten as MOP-2-P, but Sine fay aways wen wincorrecuy 28 MLZ ang tat 6 Just how stupi-ass Stike is aways gonna refer to it ~ i) d 4 CL That double bonded oxygen (ak.a. ketone) Is very amenable to tack and replacement and Is the Weal stepping stone to fal Predict ‘There are a vaity of methods to ascomplish thi inter- mediate, Many of which Strike is naw gonna lay on You! METHOD #1: Sirke's sentimental favorite. The one Strke has ‘dreamt about so very offen, This method invoNes taking hydrogen peroxide and formic acid to form a temporary intermediate which is subsequenty hysrolyzed with sufture acid 1o give the ever- lovely ketone, o53-sing, ts 20 ean) do and he resus are aoeoutly prov Gite! The poducon of MO-POP or PSP sing ts meod fas ‘en previnany taser (8.9]oxcapttat Stee gong to oe Seibel things, You krow, thse fe ouan tng that over soon {9 wo tt way io OMe Seco Dik avays aise alto sess tothe noe chert. re rome scahoe a 9 woe Mp-P2P magnetic st plate. nto the flask is poured 340g of 30% hydrogen Deroxlge (HO, always store tnis chemical inthe rage er wl degrade over time) and 15000 of ‘55% formic acid. The formic acd fumes are immensely overpowering when the stuf being transfered to {he ask but as te sown stats tof ‘hit tha foraie wen avant a ‘much "and will barely be. noticed, ‘324g isosatrle (or 2969 propenyi+ benzene for. meth) and "*000mL ‘acetone are mixed in @ PP container fd then poued ita a separatory funnel whichis stuated as shown in figuie 8. The avelone soluion is added drop by d’op into the cold formic salon eo tat the tempera ture stays between 10-20°C.. The femperatue wil stato rise @ litle bul the ee bal well locked and the dipping is consraled so thatthe temperate stays below 20°C os (Figure 8) ‘The coor of the solution wil start off clear t pale yellow, then wi tum orangy as the cripping continues, After about 200mLs of sc, Aion the chemist wil note al Ue temperature Wont Hee 40 ‘much ifthe dipping Is increased. When addon is complete the tmermometer and separatory funnel are removed. A pisce fol laced aver tha onening of the ack and the sekuion alowed (e Stir vemght. The solution is reddish erange alter the addition, Fo swe We ip atideu 10 tte ee tay and Me solution, as are ‘ovemight, wil eventually come fo room temperature asthe lost of the ice mets anay, The next day comes and the hung-over chemist wakens to see a dak red solution sting sway. In some cases Where the chemist hhad made an enormous Batch of thie aut thers may be sean a ‘mall mass of erystaline preciptate at the bottom of the fask me it amay ns ree step. ne ce Ist hd made tis ina fa-botomed flask (wrich she really should ‘have for convenience) then the ice tray ie removed, the Mask re- tumed to the st plata, = ditilation setup attached, and the ee fone & vacuum dstiled ‘rom the flask. Alter al the acetone has e2me over the chemist can proceed in two cferent way One way isto just keep on dtiling the solution unt all of the formie {2c10 nas been removed. The chemist knows that just about al the formic hac hecn amar ena te oom of ties black liquid remaining inthe reaction flask and hardly any clear forme acids diping over ito the collection ask. If one were fo Swit the reaction flask, the Eauid wil aopear syruny and ind of Coat the sides of the flask. This is more evident when the flask oak. A quick sniff of the flack may indiost that sore formes stiln there, but shouldbe too minimal o be af any concern “The problem with removing faraa amounts of formic art hy ait lation Is that ittakes a long time todo so. Really big batches can {ake an entire day to det S019 zooond option 10} afte: removal ofthe acetone would be to cool the formie acd soltion then ex: loot Ure wie ting wn ether, tne black ether layer i then washed with an ice cold 5% sodium carbonate (NaCO>) soltian to neutralize any formic ace that was camed over, then washed -55-heavy mass just as would have been attained by removal of fr- mic aed by cstiapon except tat it was done n'a fracton of the ime. Ce thing toad about this alemative is that it does rot al- ‘ways work for everybody. There can be some heavy emulsions fang, sometimes, the product forms some weird, heavy bal oft ‘This is best ted under stct adult supervision But it may not all be bad. The following is a Hive post by ‘Quits’ teting people ether extract: “1 yu mata the foe 0 mt wth 9% MAOH te Iara ‘etre ut nosy. takes <75 af 25% NaOH to mautelze he Sorter Sd o6tarn: a tno sory fa tor you hi on 45 edt voy, crt couse fin ony fo 8 (ae vu Santen ack nat to wot WEN DSM. of Ss to the Dt an sone prac floats on ie fon o you setup wh ee yre Barton yee wen SUNS er bat Finate loge wci Ether way, the chemist a gong to be staring at black syrup In the bottom of her flask. Into It she pours S00mL methanol and 200ml. 15% suluie acid soluton. Ifthe chemist does not have 2 processed in batches. As soon as the suifurc eoluton hits the Imetharovpreduc: (oxime) layes the heavy black ol wil form beads fad sink fo the bottom. The solution itself will get kind of milky and hazy. Now all the chemist does is slap a condenser into the fal jist Rea fig. Ta and roe for toe nut AM sich tn, the sdlution is allowed fo coo! downto room temperature. Now in farge batches lhe lies and tose Una are even tiger than tis ‘one its lust not feasible to extract all that auld with solvent to re- move af the ol. ust about all the os siting a the bottom ofthe ‘ack. ‘So the chomiat decant (pours off at much of the water a5 possible, adds fresh water, stirs, decants the water, adds new fresh water, etc. Thiee wastings of water should fenove sy ttaces of H:SO, let inthe ol -30- would extract the whole H:SO,/oil soluton with ether, then Wash the ether wity water. So the Of (ahich Is NOW MDZ, by te way) is transfered to @ small las usina ether and acim ce tiled (The ol ssl very black wth contaminants which need to be amaued) fer all the etyer and water have come over and the receiving flask has been exchanged witha clean, new one, i may seam ike a elerity for the ot fo get Mat enaugh to come Over But, evertuaty, te clear velo al rot wil start ecansing vn the glassware and ino the condenser, About 250g (60% 70%) of MO-P2P wil come over. The chemist knows is time to stop dst ting when the 0 fow starts to get ails orangy. ‘The MO-P2P produced here is very pure ard is sutabe fr ute in ‘any ofthe final product conversion recipes “HOT TIP #1" Distitation is sluays the most reliable way af separating tinge ftom complex mirtures such as releving aur P2P from its annoy lng: lack contaminants just tke wat was done aoove. But wouldn't be nica i there was another way t0 do it for thove vath- ‘ut a dstlation apparatus or who just dint have the time to ds- ti Well ehere aetaly is sucha way, and works fabuovely Fo yous Greniniy nave beer using sootum cxsunme (tat 18 BISULFITE not BISULFATE) to actualy erystallze a ketone out of soluion inorder to separate it As t 89 happens, our hapoy ite MO-PIP ie a ketone. And when an oil miture coctaing i mixed wit a saturated solution of sodium bisulfite (NAHSO,) the MO-P2P crysiazes out as a Disute action prod can then be eas separated by fran, Here's how i goes, where one would normaly apply dstlation, this fs te point where the chemist wit use the Bsulite. One shoul not ty this Method unless the a [srd of mast solvent. In the Mathad #1 above. one ld apply i after the ether fem the final extraction hes been moved by boling or eietlaton (Vee, some setiaton stil ap- ”lies). In the methods to come, Stike wil et vou know when ane done ‘Anyway, one has the P2PIcrap ol right? Right Next one makes @ ‘saturated saclum Diulite solzion by dissolving as much soa bisulfite as wil dssolve ina given amount of water (say, 100m), Now one adds the MO-P2P ol into some ofthe saturated soluion ‘and ste for 30 minutos, The temperature of the reaction wil rise ‘and a big old mass of P2P crystal wil form. People often say that the exyetas 0% Ike chiexen ta Nose crystas formed because the bul from the sodium bisuift latched onto the ketone of the P2P to form a precipate. And since the PP is probably the ‘nly ll component witha ketone tis gonna be the Ony thing any consequence that crystalizes. “The soutinn salen to eal andthe enals of he P2P-bisutte Addtion ‘compound are then separaied by vacuum fitraton, ‘red mls of ether, DCM or oengene, The iter cake of MD-P2P-bisutate Is processed by scraping the crystals info a ack and then 200ml of shor 20% saci carhonata saline 10% HCI solution are added (HC! works best). The colton is Stired for angtier 20) nutes during which time. the IMD-P2P-bisulite complex wil be busted up and the P2P wil re turn to its hapoy ol form. The P2P is then taken up with ether think ofthat?! “This procedure can be apoted io mast P2P mixes but i especially effective on the methods fo follow: However, in super clean meth ‘ode, such a2 the PAC, below, where lis of isosafale is. pro- ‘duced, the iso byproduct can interfere with crystal formation Someone. Wnols-hot-Stine once foun thal wher at appreciable ‘amount of osafole was formed to the detriment of MD-P2P. the Ol screwed up the crystal mati dsalowing it to form, Confused, the chemit ted to rescue the uncrystalzed oll from the aqueous solution by extracting out the ot ty ofher things. But when the solvent hit ine soluton, the P2P crystalized out. Go Myre? The ya DSEn de to the sent so the sosatce which gave the P2P a chan sonnet See ot i ets cen one Saturated sodium inde soit tat ais Contry ie oo scierborey tras nem ies Soh Sariatac ne pene ‘Prepare a strate stan of soon but ot temperate tom 400 ott yd etn She TOM ot str ao roqates ene te ote of een treat wih 7 pr cnt ots wets esfes {© elves ears mean shee ee athe wat (ba am) sus ea oreo wie, Ether pure squous or aqueouatiertsoltons w {wai up tte peterence oho chemat ox mations tee Just to mae one tel moe secre, tare site kore {hth the Bitte satin to see thay got gts Seer Se of that ketone knoum as acetone i ‘he satrated sopaon es wale the eneiaisrow. htt now chomaiy oath ‘ow nen, there ae some chemist that rely on bist eso oe [ Bhvacal searin al tthe atone eon on cage hems, ang some mathogs, se ighuly see sneer eee {her Ketoces wave pices nh hah Ye and ear separation lent necessary ta xt aren thay, ea ons 28 woul 3 ie fo ron for sure at whl trey eae aoe P2P. Ths hse proved wan he me ef ae ani to koow if what they made fe P2> a sha ae teas foes ou in ne sorted We SSttes aa coe uh Wrysas form. ene has Kelana ira oe usted happens. ve (Gre, can even use this test as a quanttatve measure, The chem 'stcan weigh Gg o soot ner P2> product erystaize k and weigh -59-thelr product i honey, and how much is not. Get i As Strke hopes you ean eee, tis simple sodlum Dist fo! as an enor fro amount of potential for helsing the evl chemist out ‘One final thought. Ste found thet there are a fot of companiee that do not sel sodium bisulfite (NaHSO:).n facta lot of compa ris ist "sodium bisute’ i her catalogs out tel the reader to see chum maha! nator’ aatien that ic tha aly fm of tis ‘Compound they cary. In other words, alot of companies sell so ‘gum metabsulte (Ne,9,0;) 95 an acceptable alternative to the ‘other. The Merck Index even says about sodium bisulfite that “he {sooium] bsuit of commerce consists chiefly of sodium metab fui, No,S,Os_and for all practical puvsns pnssasses the ‘same proper as the true bisulle”. What this meant to Strke was that metabisutre would work just ws well So some was pu ‘hase anced. And itreall does work ust the same! METHOD #2: Without a doubt thief the curent word favorit for making P2Ps. This method Is known asthe Wacker oxdaton and Involves meng savole (or any oter aiytbencene), paladin Chloride, cuprous chloride and dimethyformamide in an oxygen ‘atmosphere fo get MO-P2P very quickly and in a totaly clean ner (18, 12 ‘also a very nee foviow in rot. #13 Strike ranked t #9 in the Top en tom tne nt earton oecause Sick dint think pope would te atthe idea of using such an expensive catayst as PAC, Steet chemists are often tightassed tinen ts ie last tiny they should be when & somes tp tduetion” But this has not been the case wi this procedure a Strike has happily found out A $7-00-S6.00g, POCis ws sti prety Drsey but tha hae not honn a deterrent as many chemists have ‘aun. Nor should tbe. This procedure works so well that t wold Inrack, 8 Supra Not fo UO simul vie apy wr no 3 (redkted, Soensed research lab. The following is what vote about ike fst SeN ‘sosatole resp pans tra wot stn. nase See Sina enacts aoe Siete cee eater careers ra ec stn thn ee Tce Grant Gages ewe poe te Se al i ee aa en Sig’ eect ene hae Se Sc ah ip Rates Serre surety ose Br Sekirei basalts Om ee ete wif in tp oat erat an srt ure (which this one is going to have), Sike knows! Stike sn tne anata th seh is ee eg as tunnel a8 explained nthe How to Make seston a bis book, of -6iton ‘The pressure Is goina to come from oxyaen that is applied to the system using a balloon. Pure oxygen is easy to get. The chemist ‘can got from the neighborhood epeciaty gaa eylinder company for she can plow trough the grannies down atthe local pharmacy Sha gets smal, personal se Doe tor. Ie oxygen fs en ‘anti no hn tek wale eral Bann ha an ae Uy. (Fig 100) {Fig 106] ‘od So, 1009 of safle Io thw aden nna 8rd sng roan te foncon fav ave 1009 of FeO Og CuCl ond Dink of atnce naytgarie aie nang Se ‘and 37 Sm DE)” Omeyfocnamide OM) B She ihe ached cham’ eeu a Kelnpomamise a. DMF is a camman. legal eaten eno Task Deng Used then the openings on top ofthe addton funnel and the ae ced nock ofthe flask ave plugged wih stoppers andthe sspors secured in place with wite or strona tane. With everything eto ‘he chemist fis up a balloon with oxygen, pinches ft closed wise het fingers, wraps the end over whichover opening is appronens {and releases. This setup can look pretty cool depending on nat ‘nd of Belin the cheenist enose, Maybe one ot the thes tear ‘eliptcal kind or one with @ ducky orintnd nm Anyway, ail that pure oxygon has infitraied every part ofthe en closed system and the solution in the reaction flask is alowed ta Sti, exposed to ai that Oxygen for T hour At fist the soliton te brownish black, but as it absorbs the axyten over that hours ume ‘twill tam an lve green. After thr ifs te for the chemist o add the safole slowly over a 20min peru Ax the Sar I Dong ‘dos it wil start to ‘ake up all that oxygen caus tre oalaics iy tum 1sex again (snows that things are working) but forthe ‘dalton is complete and the snfrole hat boon converted. to MO-P2P the palacium wil again start soak up the remaining ‘oxygen and tun groen once wgatn. The wolaton remains sting st ‘om temperature for 18:24 Nour. If the Daloon loses significant volume uring tne reaction, one just fle up again. Notting bad wil happen. 7 anes a FF comainer ot 1800mL cold 3N HCI out ofthe fridge and pours the contents ofthe reacin fast foto t. Ine mire is sired a ite ang extracted 3 times with 400mL nortins of ete DCM ar thor "The ene th Ure seeds {o be added here is that the OOM extract needs to be washed 210 5 ‘mos with water. Many bees have reported trat ths 10 dduces/prevents an emulsion from happening inthe next step. The SoWent s then washed with 200mL saturated sodium bicarbonate (MalCO.\) enktinn tno ne fed Neo swiss Technically the washings can be skipped, but ether way the SO! vents going to be died througn soaium sulfate infer paper and the sodium sufate washed with atte extra snivant jst ar de Sentbed inthe methodology section of this ne book. The sovent 's thon removed by distilaton loaving what should amount to <6.‘stiling ask. (Oh boy! Hace's anctner case where there is a couple of similar boting oils thatthe poor chemist Is going to want to separate, ‘Again Sirke's gong to say that tho best way to do this without {akcy separation celumns Is going to be to alow that the fist riots ofl that cis over fs going 10 be mostyissafroe ns tha mat of the lear il that comea over is aging to be the IMO-P2P. Sirke has never been a believer in predicting the pre- UUse temperatures that something comes over at rolatve tothe Dull of vacuum or the size of the diilation spparatus. It varies foo much and Ie never apptcable to any given circumstance. ‘Shike Knows thrae things i instances tke tis: 1) solvent always ‘comes over first at low temperatures and in a very rapid manner, Zhite tsosulcle starts 10 sionly 1 over at about 170°C at regan ‘acum who the hel Knows what that is?) 3) ater about a 3-5 UJogree Increase in temperature (usualy no Increase is nowceaDe) formers impertanty, afer about 510ml of ol has collected then its time to suiten Tasks and start to collect what is assumed to be the Mo-P2P._ in Uw etd, ie chonnist should just folow her nose. Does th fist few mL of ollsmel strongly of icone? Does al the Fest ofthe ol ot?” Strike cannot answer thes ether. The 1sosa- foo fasion wil em Ske leorioe but MD-P2P aiuaye armel dif ferent ceive to the type of reaction itis borne from. Pure MULPZ> govsnt nave that sony se ad ver voualy Se ‘overpowered by Impurtis that wil aways cary over wth I from the reaction t came trom. So MD-P2P that comes from a reaction Using forme aod er morcury comaaunds is gong to smell a Sia ‘ferenty than one that came fom a reaction using pallu. However ine distinction Oetween Isosatrorsarule and MO-P2P ‘Site event In the end, alitie of one inte other isnot going to hurt tangs mc. ‘Of couse the chemist may wish to forego purifcaton and separa tion of he two femaming ols by dstlaton are opt for the sodium hisiifta pracedire deeerbed eatler. That particular method Is perfectly uted for ths situation. Perfect “6 sing oxygen Datum is ud Une CUP of 168, hen there ways 10 supply the oxygen without itt has been demenstrated, Ihatusng anon (Contoqunone) can accompah te sane hing 0 3 To do tri one re all the ingredients, including the stro ‘and quinone. stirring in the reaction flask except for the water that os ed wah tne Bhar wats gong 90 et fe ' placed in the adon funnel and aint the reactor ee ‘Another oxygen source can be that of 30% hydrogen perosie a os eee eye my that te agunous OM i made wit 20% hyeropn pec br ‘satil, To decrease that 24he span of incubalonstiring one Con: Tin te ent reatan st 8070°¢ tom th bos of nason inntercay een cnmiae nots ‘more and refi condenser Arata such canbe age by Seema oraicetenrmea (ae ioe Stace ea anita yo 0 anynay, hat was wat Stk od every the Poop tha an with een‘ camo ip wht ame Vay ie ‘eating observations of their awn since then. The foloming an fcenin the Pal metas contbatd by or goss frend TOK a hal Ske knows of TOR she seers w 86a sey nooo Blshed, cat and tae ches ina ewn ght Nee oe Bo ete, tay to be caring aoe “saninaea my ats en ad went oer o her campoun 8 Crt at coun on wha sha Sart Nor ares fo fducatonal nature and so should the folowing bo consid 2s The Wacker Oxidation a.k.a #3 0 10 (mest foo! prot ofthe ot) “68‘The folowing is her interpretation, simplified to ts MOST BASIC FORM, forthe layman wth litle experience: First she ists tho equipment, next the reagents. Also, noted are Ine nook’s quan ana nar aroam of a 8x scale up: Equipment for Sx scale: ase One Equipment lor at tom Ras (single 24/40 nec) 4 hacen hea nap ura) 1 tier eden fine! (240) 1 Yoon st bar 4 hea ty balloon {rol of ecto ape Suppor sand an lamps ‘nus ie oeam scae ‘laste fine! Phase One — Sr ecaleup Sara 200 grams a0 prams Patedum Chore “Bterams, fasorams Ciprous Chnde” ———_S00grams ‘oerams oie iets satomis Distt 120 a125mus e25mis Total Synthesie 1 oylinder of pure O, 2 above reagents (0k te sara ana 14) ort reagen) oro ihr pr messured actin The fat is SocuRty eamoed into place onthe magnetic stir Aad the DMF and sO.” Start String. and than alow ext the palm chor and eyproua Chior yeu add the powders est thon te igus you have ‘problems wth to sr bar tmang 8 race fo Sn ‘Now you have the DMF and HO string away with the PaCh and =66 = uci eae. meer te clan head adapter no tho fask Be Sure 10 anal See vac-gmacn in rej" Pass te eae {unnel the contr ho. Ad the 800 grams of sated othe fan, al ut dant sat aad dot sterg sour Mot ae Baloo i ih “Shasta sha Med un boty oe dont Dow up. “Corety tach he ballon To The rr ‘00m hal anh lita steptor and thon TAPE x wee re leakage. Frise of you Pt dont have atacs 19 Sak. 23 yanoars, acre baton One alien tea wil wor This was deseo tho baak Tin Sythe pages 921038 You ot the solution sti for 1-172 hours sot absorbs as much O, 13 possible before you start aazang he safle Everhing is kept {at room temperature fortis rreeadira The sizing soln foe Very dark, almost black n cote. Now slowly ad The safote fom the at @ fhes ebwa sintes fOr me S00 ‘rams to dio in. There 1s no noteeabia reaction as the safe \igpad xo tne string solution. Onea this 's completed ol fair ‘away forthe next 24 hours Ne: In her eam, ss haces fg balloon at the 12-hour mark. ft has gone down in size a8 O, ‘being absorbed by the sting solution Se mated another bal. Joon, removed the one that had been on there for the nas #3 !nours ana piacea ine new, ful ballon on the open hale. Tape or Wire #30 there's mo eatnge Te rset Soe ‘mosphere while the process fishes (excessive, yes, But cheap ‘and imply). Se noted that eter 3-4 hours of stig the sation ‘changes trom @ dark almost black colar fo a dark Sea green ‘anc civ green in cote. ‘Alor 24 hours, the string is stopped. Now its time fo fiterout the Cuprous Ciinide, wich 's one oF the mo sight nulsances re garding ths procedure. Note: fora! abt Paladins hina ‘recovery, 8 feo complex forthe simply ofthis procedure and Burchasea frem 2 photo suppor i shouldnt coat more tha $5.50 er gram. Weil cal this next pracess Phase Two. Phase Two. Equloment (Vac fiterina) vacuum pump oBuchner funnel Vmatman ter paper 4 fatter teing Mask Heavy Walled! ‘Suppor sands and clamps Phase Two -Chems NHC! Book eale for 1500 mis, on te dx scale up she used ‘Silica sand (white, steriized and washod) or caire ‘Methylene Chloride ‘There are two ways one ean tf fier this solution before acii- cation. Fist, Set-up your vacfitr flask with vacstrep, Buchner inne! & vae source ano start ene tering process..A Sx scale up tl take about 6-8 hours (0 fiter The cuprous chloride is In sus- pponsion and it aimos! completely clogs the itr paper making the process painfuly alow. Sho found @ motos that works fity wall fand reduces the fiter time to about an hour. Setup your Vee-ftering as usva, moisten te fier paper wih @ ue Ho, then ppoura isinch thick layer of saniizad ard washed while siica sand ‘nthe fitr paper. Moisten the sand witha small amount of HO. Feely Ure vacuity tha Sat-up and thon stort pouring te zoltion ‘ight into the sand The sand wil keep the cuprous corde from totaly cleggng the paper up. Calle can De used mn place of me and Colts ia far ai is avaliable wheraver five chemicals are S01 IfS a standard and unwatched faoratory tam, Colte works ing siniar fashion as the saonl. Vile sion sin 8 roacly avak- fabio without having fo deal wih a chenvfab supplier Place the fitered igus info 4 PP cantainer and add the appropriate amount SEAN HEL She slime # ith wonen pal far 8 fo mints ne souton i ray ror enroute i fe dist via ite used DCM and troke tinfo 4 extractions of about 1600 ms gach (she had @ 2ilter separatory funnel). Since DCM goes to te bottom, a Soparatony funnel isa must Buy or ake ops. Tha extractions ‘Should go without any problems, 25 thera isnt any emulsions £0 ontend wit "She used 109 mLs of DOM for exci! extraction, <0 satin Bearhnia Ts wasting seat ncessy te 80 can be spped DONT), The poten ait {hs i the othr nuanen ne pcos) tats sean an {amuision coven tom th wash nsuvain Ie eis nls of tho traction The eat woy ts dels 610 VEO to mass. "Your id yours of tho scum and boat the emt Ito a art 0 0 sparta. Ow washing son Sedum chore, then once wh fresh HO. Now the ext is ‘nth sour sate. You ae ro00 for Yocum Deaton The DCM extraction shoul be adeno dak rnin ne Phase Thran -Fauipment (Vee dition) Vacuum pump VacuunTap setap Heat Mane with haat controfer Grnot pate with ot bath {Balter boing Waok (round er 9at bottom) ‘Sway adapter (si hoad) 2440 7 West condenser Vacuum adapter; condenser fo receiving ask (24/40) 1 elitr round a lat Nask (sod for receiving ket) 4 thermometer adaptor (24/0) 1 thermameter 10 0 400 C. Fut vor arr nour Misc iting fo nook water ines vo ‘Aluminum fi (o wrap Nask & sil headinsuation) Support stand & compe Washed & dried DCM extractions Set-up for vac-station She wraps the flack an stil howd with ‘aluminum fo ta act as on insulator Speeds up the distilaton process: Bogin fo heat the DCM extraction sowiy der maxim <9