S. A. Richards, J. C. Hollerton

Essential Practical NMR for Organic Chemistry (eBook, PDF)

• Format: PDF

Produktbeschreibung

Essential Practical NMR for Organic Chemistry A hands-on resource advocating an ordered approach to gathering and interpreting NMR data The second edition of Essential Practical NMR for Organic Chemistry delivers a pragmatic and accessible text demonstrating an ordered approach to gathering and interpreting NMR data. In this informal guide, you'll learn to make sense of the high density of NMR information through the authors' problem-solving strategies and interpretations. The book also discusses critical aspects of NMR theory, as well as data acquisition and processing strategy. It explains the use of NMR spectroscopy for dealing with problems of small organic molecule structural elucidation and includes a brand-new chapter on Nitrogen-15 NMR. Readers will also find: * Strategies for preparing a sample, spectrum acquisition, processing, and interpreting your spectrum * Fulsome discussions of Carbon-13 NMR spectroscopy * Practical treatments of quantification, safety procedures, and relevant software An ideal handbook for anyone involved in using NMR to solve structural problems, this latest edition of Essential Practical NMR for Organic Chemistry will be particularly useful for chemists running and looking at their own NMR spectra, as well as those who work in small molecule NMR. It will also earn a place in the libraries of undergraduate and post-graduate organic chemistry students.

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Produktdetails

• Verlag: John Wiley & Sons
• Seitenzahl: 288
• Erscheinungstermin: 22. Dezember 2022
• Englisch
• ISBN-13: 9781119844815
• Artikelnr.: 67239219

Autorenporträt

S.A. Richards and J.C. Hollerton The authors have worked in NMR for GlaxoSmithKline R&D for over 40 years each, solving organic chemistry structural problems supporting synthetic and medicinal chemists. This work has required the inference of structural information from complex NMR data as well as the design of experiments to test structural hypotheses. Their breadth of experience includes instrumental, chemical, and informatics approaches to answering those important structural questions.

Inhaltsangabe

Preface xiii

1 Getting Started 1

1.1 The Technique 1

1.2 Instrumentation 2

1.2.1 CW Systems 2

1.2.2 FT Systems 3

1.2.3 Probes 5

1.2.4 Shims 6

1.3 Origin of the Chemical Shift 7

1.4 Origin of 'Splitting' 8

1.5 Integration 11

2 Preparing the Sample 13

2.1 How Much Sample Do I Need? 14

2.2 Solvent Selection 15

2.2.1 Deutero Chloroform (CDCl3) 16

2.2.2 Deutero Dimethyl Sulfoxide (DMSO) 16

2.2.3 Deutero Methanol (CD3 Od) 17

2.2.4 Deutero Water (D2O) 18

2.2.5 Deutero Benzene (C6d 6) 18

2.2.6 Carbon Tetrachloride (CCl 4) 18

2.2.7 Trifluoroacetic Acid (CF3Cooh) 18

2.2.8 Using Mixed Solvents 19

2.3 Spectrum Referencing (Proton NMR) 19

2.4 Sample Preparation 20

2.4.1 Filtration 21

3 Spectrum Acquisition 25

3.1 Number of Transients 25

3.2 Number of Points 26

3.3 Spectral Width 27

3.4 Acquisition Time 27

3.5 Pulse Width/Pulse Angle 27

3.6 Relaxation Delay 29

3.7 Number of Increments 29

3.8 Non-Uniform Sampling (NUS) 30

3.9 Shimming 30

3.10 Tuning and Matching 32

3.11 Frequency Lock 32

3.11.1 Run Unlocked 32

3.11.2 Internal Lock 32

3.11.3 External Lock 32

3.12 To Spin or Not to Spin? 33

4 Processing 35

4.1 Introduction 35

4.2 Zero-Filling and Linear Prediction 35

4.3 Apodization 36

4.4 Fourier Transformation 37

4.5 Phase Correction 37

4.6 Baseline Correction 40

4.7 Integration 40

4.8 Referencing 40

4.9 Peak Picking 41

5 Interpreting Your Spectrum 43

5.1 Common Solvents and Impurities 46

5.2 Group 1 - Exchangeables and Aldehydes 48

5.3 Group 2 - Aromatic and Heterocyclic Protons 50

5.3.1 Monosubstituted Benzene Rings 52

5.3.2 Multi-substituted Benzene Rings 55

5.3.3 Heterocyclic Ring Systems (Unsaturated) and Polycyclic Aromatic Systems 57

5.4 Group 3 - Double and Triple Bonds 61

5.5 Group 4 - Alkyl Protons 64

6 Delving Deeper 67

6.1 Chiral Centres 67

6.2 Enantiotopic and Diastereotopic Protons 72

6.3 Molecular Anisotropy 73

6.4 Accidental Equivalence 75

6.5 Restricted Rotation 77

6.6 Heteronuclear Coupling 81

6.6.1 coupling between Protons and ¯13 C 81

6.6.2 Coupling between Protons and ¯19 F 83

6.6.3 Coupling between Protons and ¯31 P 85

6.6.4 Coupling between ¯1H and Other Heteroatoms 87

6.7 Cyclic Compounds and the Karplus Curve 89

6.8 Salts, Free Bases and Zwitterions 93

6.9 Zwitterionic Compounds Are Worthy of Special Mention 94

7 Further Elucidation Techniques - Part 1 97

7.1 Chemical Techniques 97

7.1.1 Deuteration 97

7.1.2 Basification and Acidification 99

7.1.3 Changing Solvents 99

7.1.4 Trifluoroacetylation 100

7.1.5 Lanthanide Shift Reagents 101

7.1.6 Chiral Resolving Agents 102

8 Further Elucidation Techniques - Part 2 105

8.1 Introduction 105

8.2 Spin-Decoupling (Homonuclear, 1-D) 105

8.3 Correlated Spectroscopy (COSY) 106

8.4 Total Correlation Spectroscopy (TOCSY) 1- and 2-D 110

8.5 The Nuclear Overhauser Effect (NOE) and Associated Techniques 111

9 Carbon-13 NMR Spectroscopy 121

9.1 General