AKIRA Guide to MDMA Synthesis (Annotated) http://www.akirahcl.net/mdmaguide/index.

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AKIRA Guide to MDMA Synthesis (Annotated)

by Jimferd
[email] | [Return to AK IRA. HCl] | [forums]

This guide is based off of the MDMA synthesis guide found here, by Bright Star and here, by Dr. Drool. These methods have been modified to work better, and more information is provided than is given there.

Before attempting any of this, make sure you read the Notes section at the bottom for helpful hints, tips, and such.

The Synthesis
Name: MDMA )
IUPAC Name: (3,4-methylenedioxymethamphetamine
Formula: C11H15NO2
Molecular weight: 193.25 g/mol

Apparatus:
Distillation Apparatus
1 x 1000ml RBF
1 x 500ml RBF
1 x 250ml RBF
Condenser
Distillation adapter / head
Thermometer
Stand
Clamp
Hot plate / stirrer combination
Magnetic stir bar
Aspirator
Boiling Stones
Distillation tubing (12' total)
Silicon gel
Pyrex measuring cup x 3
Scale (.1g - 1000g)
pH Meter

Chemicals:
Safrole
Dimethylformamide (DMF)
para-Benzoquinone
Palladium Chloride (PdCl2)
Methylene Chloride (DCM)
HgCl Salt
Epsom Salts (MgSO4)
Aluminum foil
Hydrochloric acid (HCl, 31.45%)
Isopropyl alcohol (IPA)
Sodium Hydroxide (NaOH)
Ammonium Chloride (NH4Cl)
para-Formaldehyde
(peanut) Oil
Acetone
(para-)Xylene

Procedure:
Distillation of Safrole from Oil (if necessary)
Procedure:

1. Distill under vacuum for 4h, using <300g oil in a 500mg RBF
2. Record temperature at which safrole begins to come over
3. If temperature exceeds 160C, the vacuum is malfunctioning and needs to be reconnected. Cease heating, redistill.

Expected Yield:: 66-80% depending on purity

Formaldehyde + Ammonium Chloride ------> Methylamine.HCl

Procedure:

1. Prepare 500ml RBF for vacuum distillation

2. Add 108g NH4Cl, 120g p-formaldehyde (molecular ratio 1:2), 320ml HOH
3. Heat slowly with boiling stones to prevent bumping
4. Turn on condenser
5. At 80C, solution will become clear. Let stand at 104C for 4h, allowing distillate to come over.
6. Slowly increase heat over the course of 30 minutes.
7. Vacuum distill, cool distillate in ice/water bath.
8. Filter off NH4Cl crystals

Expected Yield: 80g methylamine.HCl, 80%

Safrole, p-Benzoquinone, Palladium Chloride reac t to form MDP-2-P (Wacker Oxidation)

Procedure:

1. To a clean 1,000ml RBF, add 300ml DMF, 50ml HOH, 120g para-Benzoquinone
2. While stirring slowly, mix 160g safrole, 50ml DMF, over the course of 30 minutes, to solution.
3. Increase stirring speed, stir for 7h or until temperature has stabilized.
4. Flood with acidic solution (50ml HCl in 1.5l HOH)
5. Use 4000ml separation funnel
6. Decant aqueous layer
7. Wash: 2 x 150ml 10% NaOH
8. Discard NaOH layer
9. Store in sealed container in freezer

Expected Yield: 40g MDP-2-P

MDP-2-P, Methylamine. HCl react to form MDMA via Al/Hg Amalgam

Table of Boiling points:

SUBSTANCE BP [* C]
DCM 40
HOH 100

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DMF 153
Safrole 232
MDP-2-P 292

Procedure:

1. 20g 2cm x 2cm aluminum foil squares were added to a 500ml RBF with 325 ml HOH
2. Add .2 g HgCl
3. Let settle until fine bubbles / shiny spots on the aluminum form.
4. Pour water into separate RBF
5. Add 350ml HOH, agitate for 2min, repeat
6. Quickly decant as much HOH as possible within 10s, leaving Al and as little HOH as possible.
7. Add 50g methylamine.HCl in 300ml 91% IPA, followed by 40g MDP-2-P in 50ml IPA.
8. Drip 25ml 25% NaOH over 10min
9. Allow reaction to occur for 6h, maintaining a temperature of below 60C using an ice/water bath
10. Let stand until temperature stabilizes, cooling as needed.
11. Add 25ml 25% NaOH, stir, let stand for 30min, repeat.
12. Decand yellow liquid; mix 200ml 91% IPA, decant, repeat until no more yellow liquid forms
13. Dispose of sludge safely, taking care that mercury is contained within
14. Evaporate IPA with non vacuum distillation, adding boiling stones.
15. Vacuum distill. Remainder of IPA will come over at 35C; ensure all IPA is completely removed before proceeding
16. Add 470ml HOH with 30ml HCl, agitate
17. Add 30ml DCM, shake, let stand.
18. The top (aqueous) layer contains the MDMA; wash with an additional 30ml DCM. Discard DCM washes but notaqueous layer
19. Add 50ml NaOH, wash with 50ml DCM, agitate - the DCM will contain the MDMA
20. Using boiling stones, boil off DCM, let temperature roughly equal 50C for 10min until light brown oil is obtained.

"Dry" IPA Wash and Recrystalliz ation:

Procedure:

1. Form "dry" IPA by emptying 100ml from a new bottle, adding 100ml in volume worth of MgSO4, repeat four times, agitating after each addition
2. Mix 100ml "dry" IPA and 150ml Xylene, stir well into MDMA for 15-30min
3. Drip HCl and titrate pH to 5-6 (barely acidic)
4. Vacuum distill with stir bar once the solution is at proper pH.
5. Filter with coffee filter
6. Dry filter cake under heat lamp
7. Wash with 20ml acetone twice, stirring each time to remove impurities, dry again

Expected yield15g MDMA.HCl

Diagrams
Safrole:

Reduction of Formaldehyde and Ammonium Chloride to produce Methylamine.HCl

Oxidation of Safrole to produce MDP-2-P

MDP-2-P to MDMA

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Notes
Distilla tion Notes
If using a natural oil as the source of safrole, vacuum distill for four hours, heating, and recording the temperature at which it comes over. This is later used during the distillation of MDP-2-P. The temperature
should not exceed 160C - it means your apparatus is haywire and needs to be reattached. Very likely the tube is not forming a solid vacuum. A little silicon gel will help here or just a tighter attachment.

You'll want to switch flasks on the recieving flask once the safrole begins to come over, just so the safrole is pure. If necessary, that mixture can be decanted, to leave the purest safrole solution possible.

Methyla mine Rea ction Notes

p-Formaldehyde and N-Formaldehyde are interchangable here; either can be used so long as it is 37%. The methylamine can be store permanently so long as it is well sealed.

As you can see, this is a two part reaction - first the double bond is broken, then methylamine is formed from the methylimine.

Wacker Oxida tion Notes

At 4.5 h, the soluton should be warm, indicating that the reaction is properly occuring. At 6-6.5h the solution should be back to room temperature and stabilized. Using more than 2g of PdCl2 is acceptable; it'll get
washed out anyway and since it's the catalyst, you can't really have too much, within reason. Note also to ensure that you remove the hydroquinone as it will clog the condenser next time you try to distill. The
layer contains DCM, MDP-2P, etc.

Al / Hg Amalgam

Hg strips the Al2O3 off, allowing Al3+ to catalyze the reaction for the formation of MDMA, in a process called reductive amination.

General Notes:
Ensure you can acquire everything before you begin. It's a pain to suddenly have to run out and get something, especially if you're in the middle of a time crunch reaction like the Al/Hg amalgam, which could
potentially cause you to lose all your product, ie, bad. You can expect to spend about $1200 for your first synthesis and then an additional $200 each time afterwards.

The synthesis is, in my opinion, pretty simple. There are only 3 reactions involved. If you're careful, follow the procedure to a T, and have the equipment and chemicals necessary to do this, it should be relatively
simple.

Set up everything ahead of time. Vacuum distill water or something first, just to get an idea of how it works. Set up the distillation setup on a soft surface (bed), and play with it. Make sure the clamps are set up
right as they'll hold literally $800 worth of glassware.

The overall process, even if executed perfectly, will take a few days of interrupted sleep schedules. There are long periods of waiting for reactions to complete, and if you're going to rerun the reaction to make a
lot of product for use in future syntheses, then it's going to take even longer. The first time is going to be a challenge because you're not going to know what you're doing, but after the second or third synthesis,
you'll have it down pat.

As for colors, the amalgam should be a silver-gray sludge, and when NaOH is added, should turn into a dark almost black liquid that will emit gas. The finished MDMA product should be a pure white crystalline
solid. It should be odorless. If it smells, rewash. Having something impure in the final product could mean bad things if ingested. This is, after all, going to be eaten, so great care should be taken to ensure its
safety.

Keep a fire extinguisher nearby, wear goggles, lab coat, and fume mask. Additionally, don't wear anything you're not willing to destroy, as you're likely to splash NaOH or HCl on your clothes at some point, which
will bore holes in them. I cannot stress this last point enough - wear gloves. Buy the ones that go up to your elbows. Dishwashing gloves are not adequate. Use the thick rubber ones that fishermen use.

Buy the real thing if you can - for example, as Dr. Drool says, don't buy Jasco stripper when you can just by methylene chloride from a science supply house. Also make sure you keep your science equipment
bills under $100 each time, for chemicals, or they will be reported to the DEA. Mail order when possible; going through Canada is a fairly safe bet because it's harder for the DEA to track than if you were to
purchase it through Chicago.

When purchasing the Safrole, I'd recommend Asia. While it's going to be less reliable - you're going to get ripped off quite possibly - it's much less likely to be a DEA shell than if you were to buy it, again, from a
dealer in Chicago. The best safrole tends to come from Vietnam in the form of natural oils; also, if you can get it, you can usually get 95-100% pure safrole oil from North Korea via China.

Always work in a well ventilated area, especially when working with solvents, or if you end up using the nitromethane method detailed below, with that.

Read everything you can about how to do everything before actually doing it, or you're going to end up wasting a lot of materials. Do a dry run first, just to make sure you have things down. Do not, for example,
commit safrole oil when you don't know what you're doing, only to end up losing some.

A note about the separatory funnel - if the pressure builds up from a separation, it's almost certain to cause the plug to fire out. If you're working on a concrete floor, as you should be, this will break the plug and
render the funnel useless. Always keep your hand over the plug.

Using Nitromethane: Nitromethane can be bought in the form of hobby fuel. Boil it in a bath of oil, as it won't come over until 101C. When distilling, watch out for a bump when distilling; use a stir bar as opposed
to boiling stones or you will end up having a rough time as the solution continuously bumps. Use the nitromethane as opposed to methylamine.

When cooking epsom salts to dehydrate the, place them in an oven at 400C. Cook fewer than you think you'll be able to at a time or it will stick to the cooking pan and trouble will arise. Seal in a jar or other
air-tight container so as to not allow water to condense from the atmosphere into the crystals.

Read everything you can about this before doing it, and above all, good luck!

From the Notes of Dr. Alexander Shulgin in PiHKAL

With MDMA, the usual assignments of activity to optical isomers is reversed from all of the known psychedelic drugs. The more potent isomer is the “S†isomer, which is the more potent form of
amphetamine and methamphetamine. This was one of the first clear distinctions that was apparent between MDMA and the structurally related psychedelics (where the “R†isomers are the more
active). Tolerance studies also support differences in mechanisms of action. In one study, MDMA was consumed at 9:00 a.m. each day for almost a week (120 milligrams the first day and 160 milligrams
each subsequent day) and by the fifth day there were no effects from the drug except for some mydriasis. And even this appeared to be lost on the sixth day. At this point of total tolerance, there was
consumed (on day #7, at 9:00 a.m.) 120 milligrams of MDA and the response to it was substantially normal with proper chronology, teeth clench, and at most only a slight decrease in mental change. A
complete holiday from any drug for another 6 days led to the reversal of this tolerance, in that 120 milligrams of MDMA had substantially the full expected effects. The fact that MDMA and MDA are not
cross-tolerant strengthens the argument that they act in different ways, and at different sites in the brain.

A wide popularization of the social use of MDMA occurred in 1984–1985 and, with the reported observation of serotonin nerve changes in animal models resulting from the administration of the
structurally similar drug MDA, an administrative move was launched to place it under legal control. The placement of MDMA into the most restrictive category of the Federal Controlled Substances Act has
effectively removed it from the area of clinical experimentation and human research. The medical potential of this material will probably have to be developed through studies overseas.

A word of caution is in order concerning the intermediate 3,4-methylenedioxyphenylacetone, which has also been called piperonylacetone. A devilish ambiguity appeared in the commercial market for this
compound, centered about its name. The controversy focused on the meaning of the prefix, piperonyl, which has two separate chemical definitions. Let me try to explain this fascinating chaos in
non-chemical terms. Piperonyl is a term that has been used for a two-ring system (the methylenedioxyphenyl group) either without, or with, an extra carbon atom sticking off of the side of it. Thus,
piperonylacetone can be piperonyl (the two-ring thing without the extra carbon atom attached) plus acetone (a three carbon chain thing); the total number of carbons sticking out, three. Or,
piperonylacetone can be piperonyl (the two-ring thing but with the extra carbon atom attached) plus acetone (a three carbon chain thing); the total number of carbons sticking out, four.

Does this make sense?

The three carbon sticking out job gives rise to MDA and to MDMA and to many homologues that are interesting materials discussed at length in these Book II comments. This is the usual item of
commerce, available from both domestic and foreign suppliers. But the four-carbon sticking out job will produce totally weird stuff without any apparent relationship to psychedelics, psychoactives or
psychotropics whatsoever. I know of one chemical supply house which supplied the weird compound, and they never did acknowledge their unusual use of the term piperonyl. There is a simple difference
of properties which might be of value. The three carbon (correct) ketone is an oil with a sassafras smell that is always yellow colored. The four carbon (incorrect) ketone has a weak terpene smell and is
white and crystalline. There should be no difficulties in distinguishing these two compounds. But unprincipled charlatans can always add mineral oil and butter yellow to otherwise white solids to make
them into yellow oils. Caveat emptor.

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03/26/2009 - AKIRA. HCL - E-MAIL AUT HOR

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