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Organic Structure Determination Using 2-D NMR Spectroscopy
This book contains 30-40 quality 2D NMR data sets following an introductory section describing the methodology employed. Many other books describe the methods used, but none offer a large number of problems. Instructors at universities and colleges at the present time are forced to cobble together problems from a wide range of sources. The fragmentary approach to assembling course materials has a negative impact on course continuity and thus adversely impacts student retention. This book will stand as a single source to which instructors and students can go to obtain a comprehensive compe.
Front Cover; Organic Structure Determination Using 2-D NMR Spectroscopy: A Problem-Based Approach; Copyright; Dedicated to; Contents; Preface; Preface to the First Edition; Chapter 1 -- Introduction; 1.1 What Is Nuclear Magnetic Resonance?; 1.2 Consequences of Nuclear Spin; 1.3 Application of a Magnetic Field to a Nuclear Spin; 1.4 Application of a Magnetic Field to an Ensemble of Nuclear Spins; 1.5 Tipping the Net Magnetization Vector from Equilibrium; 1.6 Signal Detection; 1.7 The Chemical Shift; 1.8 The 1-D NMR Spectrum; 1.9 The 2-D NMR Spectrum.
1.10 Information Content Available Using NMR SpectroscopyProblems for Chapter One; Chapter 2 -- Instrumental Considerations; 2.1 Sample Preparation; 2.2 Locking; 2.3 Shimming; 2.4 Temperature Regulation; 2.5 Modern NMR Instrument Architecture; 2.6 Pulse Calibration; 2.7 Sample Excitation and the Rotating Frame of Reference; 2.8 Pulse Rolloff; 2.9 Probe Variations; 2.10 Analog Signal Detection; 2.11 Signal Digitization; Problems for Chapter Two; References; Chapter 3 -- Data Collection, Processing, and Plotting; 3.1 Setting the Spectral Window.
3.2 Determining the Optimal Wait (Delay) Between Scans3.3 Setting the Acquisition Time; 3.4 How Many Points to Acquire in a 1-D Spectrum; 3.5 Zero Filling and Digital Resolution; 3.6 Setting the Number of Points to Acquire in a 2-D Spectrum; 3.7 Truncation Error and Apodization; 3.8 The Relationship Between T2 * and Observed Line Width; 3.9 Resolution Enhancement; 3.10 Forward Linear Prediction; 3.11 Pulse Ringdown and Backward Linear Prediction31; 3.12 Phase Correction; 3.13 Baseline Correction39; 3.14 Integration; 3.15 Measurement of Chemical Shifts and J-Couplings.
3.16 Data RepresentationProblems for Chapter Three; Chapter 4 -- 1H and 13C Chemical Shifts; 4.1 The Nature of the Chemical Shift; 4.2 Aliphatic Hydrocarbons; 4.3 Saturated, Cyclic Hydrocarbons; 4.4 Olefinic Hydrocarbons; 4.5 Acetylenic Hydrocarbons; 4.6 Aromatic Hydrocarbons; 4.7 Heteroatom Effects; Problems for Chapter Four; Reference; Chapter 5 -- Symmetry and Topicity; 5.1 Homotopicity; 5.2 Enantiotopicity; 5.3 Diastereotopicity; 5.4 Chemical Equivalence; 5.5 Magnetic Equivalence; Problems for Chapter Five; Reference; Chapter 6 -- Through-Bond Effects: Spin-Spin (J) Coupling.
6.1 Origin of J-Coupling6.2 Skewing of the Intensity of Multiplets; 6.3 Prediction of First-Order Multiplets; 6.4 The Karplus Relationship for Spins Separated by Three Bonds; 6.5 The Karplus Relationship for Spins Separated by Two Bonds; 6.6 Long Range J-Coupling; 6.7 Decoupling Methods; 6.8 One-Dimensional Experiments Utilizing J-Couplings; 6.9 Two-Dimensional Experiments Utilizing J-Couplings; Problems for Chapter Six; References; Chapter 7 -- Through-Space Effects: The Nuclear Overhauser Effect (NOE); 7.1 The Dipolar Relaxation Pathway.
7.2 The Energetics of an Isolated Heteronuclear Two-Spin System.
Organic Structure Determination Using 2-D NMR Spectroscopy : A Problem-Based Approach