Lecture on 10.6 10.

12
1. Introduction to 2D-NMR 10.6
2. COSY (H-H Correlation Spectroscopy) 10.7
A.
B.

Overview of COSY
How to Read COSY Spectra

3. HETCOR (Heteronuclear Correlation Spectroscopy) 10.8

A. B. Overview of HETCOR How to Read HETCOR Spectra

4. Inverse Detection Methods 10.9 5. NOESY (Nuclear Overhauser Effect Spectroscopy) 10.10 6. ON YOUR OWN Sections 10.11 + 10.12
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Introduction to 2D-NMR 10.6

1. 1D vs. 2D NMR 2. 3 dimensions contour plot X + Y axis chemical shift ranges 3rd dimension intensity of signals 3. Evolution Phase extra time in pulse sequence before data acquisition that allows for information to be exchanged between magnetic nuclei.

4. Homonuclear 2D NMR interactions between neighboring atoms of the same magnetically active isotope 5. Heteronuclear 2D NMR interactions between neighboring atoms of different magnetically active isotopes
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COSY (H-H Correlation Spectroscopy) 10.7

A. Overview of COSY (correlation spectroscopy) 1. Pulse Sequence, etc. our outside the scope of this course. 2. Diagonal Peaks provide no useful information side effect of expt. 3. Cross Peaks (Off-Diagonal Peaks) proof of spin coupling between neighboring hydrogens 4. Requires a large number of FIDs takes a long time (30 min. to an hour, if not more) needs a computer with a lot of memory 5. Low Resolution 6. gCOSY (gradient-selected COSY) fixes issue of resolution and time length of regular COSY B. How to Read COSY Spectra 1. Figures 10.13, 10.14, + 10.15
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Dr. Timothy M. Trygstad, The College of St. Scholastica, Duluth, Minnesota

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Dr. Timothy M. Trygstad, The College of St. Scholastica, Duluth, Minnesota

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Dr. Timothy M. Trygstad, The College of St. Scholastica, Duluth, Minnesota

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HETCOR (Heteronuclear Correlation Spectroscopy) 10.8

A. Overview of HETCOR 1. Pulse Sequence, etc. our outside the scope of this course.

2. No Diagonal Peaks why not?

3. Cross Peaks (Off-Diagonal Peaks) proof of spin coupling between carbons and attached hydrogens 4. Low Resolution in 1H Signals leads to problems in spectra with numerous H signals. 5. High Resolution in 13C Signals B. How to Read HETCOR Spectra 1. Figures 10.16, 10.17, + 10.18
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Dr. Timothy M. Trygstad, The College of St. Scholastica, Duluth, Minnesota

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Dr. Timothy M. Trygstad, The College of St. Scholastica, Duluth, Minnesota

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Dr. Timothy M. Trygstad, The College of St. Scholastica, Duluth, Minnesota

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Inverse Detection Methods 10.9

1. Switches initial pulse to occur in the 1H channel, thus giving the best resolution to the 1H signals. 2. Produces a much cleaner heteronuclear 2D NMR 3. HMQC (heteronuclear multiple-quantum correlation)

4. HSQC (heteronuclear single-quantum correlation)

5. Both HMQC and HSQC provide the same information as a HETCOR, but have significantly improved resolution for the 1H signals, thus they are the preferred method for more complex and larger molecules.

Copyright 2009, Dr. Timothy M. Trygstad, The College of St. Scholastica, Duluth, Minnesota

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NOESY (Nuclear Overhauser Effect Spectroscopy) 10.10

1. Any 1H nuclei that interact with each other through dipolar relaxation processes will appear as cross peaks in a NOESY. nuclei directly coupled to each other through bonds nuclei not directly coupled, but interact through space 2. Looks very similar to a COSY spectrum. 3. It is the additional cross peaks, in comparison to the COSY, that show the through space interactions. 4. Provides 3D Information configurations and conformations 5. Very useful in large molecules. proteins, polynucleotides, biologically derived molecules 6. Example on page 614 of Pavia
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