Organic Structure Determination Using 2-D NMR Spectroscopy——A Problem-Based Approach By Jeffrey H. Simpson
Table of ContentsPART I: Background and Methods
Chapter 1: Introduction
What is NMR?
Consequences of Nuclear Spin
Application of a Magnetic Field to a Single Nuclear Spin
Application of a Magnetic Field to an Ensemble of Nuclear Spins
Tipping the Net Magnetization Vector from Equilibrium
Signal Detection
The Chemical Shift
The 1-D NMR Spectrum
The 2-D NMR Spectrum
Information Content Available Using NMR
Chapter 2: Instrumental Considerations
Sample Preparation
Locking
Shimming
Temperature Regulation
Modern NMR Instrument Architecture
Pulse Calibration
Sample Excitation and the Rotating Frame of Reference
Pulse Rolloff
Probe Variations
og Signal Detection
Signal Digitization
Chapter 3: Data Collection, Processing, and Plotting
Setting the Spectral Window
Determining the Optimal Wait Between Scans
Setting the Acquisition Time
How Many Points to Acquire in a 1-D Spectrum
Zero Filling and Digital Resolution
Setting the Number of Points to Acquire in a 2-D Spectrum
Truncation Error and Apodization
The Relationship Between T2
and Observed Line Width
Resolution Enhancement
Forward Linear Prediction
Pulse Ringdown and Backward Linear Prediction
Phase Correction
Baseline Correction
Integration
Measurement of Chemical Shifts and J-Couplings
Data Representation
Chapter 4: 1H and 13C Chemical Shifts
The Nature of the Chemical Shift
Aliphatic Hydrocarbons
Saturated, Cyclic Hydrocarbons
Olefinic Hydrocarbons
Acetylenic Hydrocarbons
Aromatic Hydrocarbons
Heteroatom Effects
Chapter 5: Symmetry and Topicity
Homotopicity
Enantiotopicity
Diastereotopicity
Chemical Equivalence
Magnetic Equivalence
Chapter 6: Through-Bond Effects: Spin-Spin (J) Coupling
Origin of J-Coupling
Skewing of the Intensity of Multiplets
Prediction of First-Order Multiplets
The Karplus Relationship for Spins Separated by Three Bonds
The Karplus Relationship for Spins Separated by Two Bonds
Long Range J-Coupling
Decoupling Methods
One-Dimensional Experiments Utilizing J-Couplings
Two-Dimensional Experiments Utilizing J-Couplings
Chapter 7: Through-Space Effects: the Nuclear Overhauser Effect (NOE)
The Dipolar Relaxation Pathway
The Energetics of an Isolated Heteronuclear Two-Spin System
The Spectral Density Function
Decoupling One of the Spins in a Heteronuclear Two-Spin System
Rapid Relaxation via the Double Quantum Pathway
A One-Dimensional Experiment Utilizing the NOE
Two-Dimensional Experiments Utilizing the NOE
Chapter 8: Molecular Dynamics
Relaxation
Rapid Chemical Exchange
Slow Chemical Exchange
Intermediate Chemical Exchange
Two-Dimensional Experiments that Show Exchange
Chapter 9: Strategies for Assigning Molecules
Prediction of Chemical Shifts
Prediction of Integrals and Intensities
Prediction of 1H Multiplets
Good Bookkeeping Practices
Assigning 1H Resonances on the Basis of Chemical Shifts
Assigning 1H Resonances on the Basis of Multiplicities
Assigning 1H Resonances on the Basis of the gCOSY Spectrum
The Best Way to Read a 2-D gCOSY Spectrum
Assigning 13C Resonances on the Basis of Chemical Shifts
Pairing 1H and 13C Shifts By Using the HSQC/HMQC Spectrum
Assignment of Non-Protonated 13C’s on the Basis of the HMBC Spectrum
Chapter 10: Strategies for Elucidating Unknown Molecular Structures
Initial Inspection of the One-Dimensional Spectra
Good Accounting Practices
Identification of Entry Points
Completion of Assignments
PART II: Problems
Chapter 11 Simple Assignment Problems
Chapter 12: Complex Assignment Problems
Chapter 13: Simple Unknown Problems
Chapter 14: Complex Unknown Problems
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