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Jan. 10
Intro
to NMR
Operation
of EFT for C13 spectra and interpretation
of C13 spectra.
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Goals:
1. We meet students
and they meet us.
2. Students learn how to
run instrument. Each group of 4 does 4 C13 spectra. (hexane,
cyclohexane, 1-hexanol, cyclohexanol).
3. The students learn
how to see how many peaks would be in a C13 spectra based on its structure.
4. The students
and make up a summary table of C-13 NMR
results (peaks, ppm, relative intensity) and associate peaks with
structures.
5.
Students learn how to look up nmr spectra on the
web.
6. Review of normal valence rules for H, C, N, O, Cl, Br.
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Lab. Operation of
instrument. C13 of Knowns hexane, hexanol, cyclohexanol,
cyclohexane. Interpretation and making summary table for 4 compounds
with c-13 spectra.
Homework.
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Jan. 12
Lecture Alkanes, cycloalkanes
.
DEPT
and C13 spectra.
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Goals.
1. Basic organic
nomenclature for alkanes, alkenes, etc.
2. Taking and interpreting dept
spectra and making summary table that includes number of attached H
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Lab. Operation of
instrument to obtain DEPT spectra. 2 known.
1st
unknown.
Homework:
Combination C-13 nmr and nomenclature.
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Jan. 17
Proton
spectra. Coupling and Integration. Interpretation of H spectra
especially coupling and integration. 2 known spectra and 6 theoretical
spectra.
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Goals.
1. Coupling.
Proton proton coupling in organic compounds.
2. Integration in
organic compounds.
3. Summary tables for
Proton spectra.
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Lab. 2 knowns
Homework.
6 theoretical structures
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Jan. 19
Substituted
alkanes. Alcohols, amines, and halides. Nomencclature.
Major Unknown #2.
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Goals
1. Nomenclature of
simple substituted hydrocarbons.
2. Structural isomers
nomenclature, structures, and nmr.
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Lab. 2nd
Unknown.
Homework
combination nomenclature and nmr
Quiz 1.
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Jan. 24
Arene compounds. Known ethyl benzene. Making
up nmr samples. 4 theoretical structures
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Goals.
1. Nomenclature of arene compounds and geometric isomers, structures, and
NMR.
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Homework:
Geometric isomers of benzene
Lab. 1 Known. 3rd
Unknown.
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Jan 26
Coupling Revisited. Coupling in carbon 13 NMR.
Decoupling
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Goals.
1. Origin of coupling.
Pascals triangle.
2. Nuclear Overhauser Effect.
3.
Decoupling. Instrumental decoupling. Exchange decoupling.
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Principles Lab. Coupled and decoupled C-13 spectra
of a known.
Homework. Coupling and decoupling questions.
Quiz 2
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Jan. 31
Carbonyl
compounds.
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Goals.
1.
Nomenclature of carbonyl compounds
2.
NMR of isomers of
carbonyl compounds
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Lab. 1 known. 4th Unknown.
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Feb. 2
NMR details. Ppm and Hz,
resolution, sensitivity, shimming, tuning, superconductivity,
electromagnets, permanent magnets. etc.
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Goals.
1. Review of basic terminology
and terminology that describes instrumental and technical problems.
2. Understanding
factors involved with resolution.
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Principles Lab.
High field low field spectra. Known 1-butanol on Unity +500 and EFT
60. Field effects and calculation of chemical shifts in
ppm and Hz. Effect of field on coupling.
Unknown 5 out.
Quiz 3
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Feb 7
Previous continued.
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Goal.
1.
Understanding of sensitivity, solution concentration,
field strength.
2.
Calculation
of energy difference of spin states.
3.
Signal to
Noise calculation.
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Principles lab. High field,
low field. Sensitivity of solution vs neat
samples. Sensitivity of instrument and field strength
4th unknown
due
|
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Feb. 9
Nuclei other than C-13 and H-1: H-2
Lecture
Notes
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Goal.
1. Basic nuclear
properties that effect nmr.
2. Spectra of deuterated solvents and coupling by nuclei with spin
=1.
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Principles lab. Proton spectra of deuterated acetone, D/H coupling. C-13 coupling to H in
CHCl3, the natural abundance of C-13.
Quiz 4
Unknown 6 out on 2-10.
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Feb. 14
The pulse experiment.
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Goal.
1. Look at the basic
pulse experiment .
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Principles Lab. Determination of PW 90.
Unknown 5 due. Should have
H, C-13 and DEPT spectra and
interpretation of them
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Feb. 16
Signal to noise
and number of scans.
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Goal.
1. Design of experiments and signal to noise.
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Principles Lab. Determination of signal to noise vs number of scans.
Unknown 6 due. Should
have H, C-13 and DEPT spectra and interprettation of them
Unknown 7. A Solution Unknown.
Quiz 5
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Feb. 21
Spectral Editing (Attached Proton Test) and 2D NMR
(Het2dj)
|
1.
Brief introduction to more complex pulse sequences and
spectra.
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Feb 23
TBA
|
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Quiz 6
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Feb 28
Review
2007 Final-NMR part
|
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Unknowns 7 due. Include
identification of solvent and reference peaks.
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March 2.
Final exam
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