Second  Edition out NOW

 

 

High-Resolution NMR Techniques in Organic Chemistry

T. D. W. Claridge, 2nd Edition

 

 

 Contents

  Reviewers' Comments (of first edition)

 Errata (to first edition)

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The first edition is also available in Japanese; See www.kspub.co.jp

Nuclear Magnetic Resonance (NMR) Spectroscopy remains the foremost analytical technique for the structure elucidation of organic molecules and an indispensable tool for the synthetic, medicinal and natural product chemist. New techniques continue to emerge and the application of NMR methods continues to expand. High-Resolution NMR Techniques in Organic Chemistry is designed for use in academic and industrial NMR facilities, as a text for graduate-level NMR courses, and as an accessible reference for the chemist’s or spectroscopist’s desk.

The second edition of this classic text emphasizes:

• recent developments in the field, with practical guidance on implementation, execution and application

• advances in hardware, pulse sequence development, and associated experimental methodologies

Contents

Chapter 1: Introduction
1.1 The development of high-resolution NMR
1.2 Modern NMR and this book
1.3 Applying modern NMR techniques
References

Chapter 2: Introducing high-resolution NMR
2.1 Nuclear spin and resonance
2.2 The vector model and pulse excitation
2.3 Time and frequency domains
2.4 Spin relaxation
2.5 Mechanisms for relaxation
References

Chapter 3: Practical aspects of high-resolution NMR
3.1 An overview of the NMR spectrometer
3.2 Data acquisition and processing
3.3 Preparing the sample
3.4 Preparing the spectrometer
3.5 Spectrometer calibrations
3.6 Spectrometer performance tests
References

Chapter 4: One-dimensional techniques
4.1 The single-pulse experiment
4.2 Spin decoupling methods
4.3 Spectrum editing with spin-echoes
4.4 Sensitivity enhancement and spectrum editing
4.5 Observing quadrupolar nuclei
References

Chapter 5: Correlations through the chemical bond I: Homonuclear shift correlation
5.1 Introducing the second dimension
5.2 Correlation spectroscopy (COSY)
5.3 Practical aspects of 2D NMR
5.4 Coherence and coherence transfer
5.5 Gradient-selected spectroscopy
5.6 Alternative COSY sequences
5.7 Total correlation spectroscopy (TOCSY)
5.8 Correlating dilute spins with INADEQUATE
5.9 Correlation dilute spins with ADEQUATE
References

Chapter 6: Correlations through the chemical bond II: Heteronuclear shift correlation
6.1 Introduction
6.2 Sensitivity
6.3 Heteronuclear single-bond correlation spectroscopy
6.4 Heteronuclear multiple-bond correlation spectroscopy
6.5 Heteronuclear X-detected correlation spectroscopy
6.6 Heteronuclear X-Y correlations
References

Chapter 7: Separating shifts and couplings: J-resolved spectroscopy
7.1 Introduction
7.2 Heteronuclear J-resolved spectroscopy
7.3 Homonuclear J-resolved spectroscopy
7.4 "Indirect" homonuclear J-resolved spectroscopy
References

Chapter 8: Correlations through space: The nuclear Overhauser effect
Part I: Theoretical aspects

8.1 Introduction
8.2 Definition of the NOE
8.3 Steady-state NOEs
8.4 Transient NOEs
8.5 Rotating-frame NOEs
Part II: Practical aspects
8.6 Measuring steady-state NOEs: NOE difference
8.7 Measuring transient NOEs: NOESY
8.8 Measuring rotating-frame NOEs: ROESY
8.9 Measuring heteronuclear NOEs
8.10 Experimental considerations
References

Chapter 9: Diffusion NMR Spectroscopy
9.1 Introduction
9.2 Measuring self-diffusion by NMR
9.3 Practical aspects of diffusion NMR spectroscopy
9.4 Applications of diffusion NMR spectroscopy
9.5 Hybrid diffusion sequences
References

Chapter 10: Experimental Methods
10.1 Composite pulses
10.2 Adiabatic and broadband pulses
10.3 Broadband decoupling and spin-locking
10.4 Selective excitation and shaped pulses
10.5 Solvent suppression
10.6 Suppression of zero-quantum coherences
10.7 Heterogeneous samples and MAS
10.8 Emerging methods
References

Appendix: Glossary of acronyms

Index


Reviewers' comments of the first edition

"This is a very well produced and nicely laid-out book.... the descriptions, explanations, diagrams and spectra given here are clearer than in most of its rivals"
Steven Firth, The Alchemist, ChemWeb, 2000

"The explanations are clear and concise... the references are well done and up-to-date. This book is a practical guide for the beginner as well as a launching pad for the NMR enthusiast. It should be found in every NMR facility."
Ben Shoulders, J.A.C.S, 2000

"The book is an excellent reference source and guide for the most common NMR experiments used by organic chemists, and it is also an excellent textbook for organic graduate and postdoctoral students.... Overall this a very good text, both well written and easy to understand....I highly recommend the text."
Rickey P. Hicks, J. Nat. Prod., 2000

"For the budding NMR spectroscopist, for the synthetic chemist with an interest in and contact with NMR spectroscopy, and also as a foundation for graduate-level courses on NMR techniques, this book is highly recommended... It is essential for every NMR laboratory dealing with small and mid-sized molecules"
Ruth Gschwind, Angewandte Chemie, 2001


Errata to first edition

The errors listed below were corrected in the 2004 reprint.

These are the errors currently known to me. Please let me know by email of you are aware of any others. Thanks!.

 

Page 4: 6th line from bottom: The sentance "Even if you see yourself the first of the above..." should read "Even if you see yourself in the first of the above..."

Page 8: 16th line from bottom: "sought" should read "sort"

Page 10: 11th line from bottom: "sought" should read "sort"

Page 15: In equation 2.4 and the associated text the Gas Constant R should, of course, be the Boltzmann Constant k.

Page 18: Caption to Fig. 2.9: "posses" should read "possess"

Page 21: 4th line: "Section 2.2" should read "Section 3.2"

Page 32: 11th line from bottom: "determinig" should read "determining"

Page 33: Fig. 2.29: small rectangle over last vertical arrow should not be there.

Page 51: Fig. 3.7(b): small grey lines to the left of, and above, label x should not be there.

Page 53: Fig. 3.11 is missing its labels and should read (a), (b) and (c) from the bottom up.

Page 54: 5th line from bottom: "..., or from poor field inhomogeneity, ..." should read "..., or from poor field homogeneity, ..."

Page 63: Lines above section 3.2.5: The use of the term absolute frequency here may be a little misleading as NMR spectrum frequencies are measured relative to the carrier rf frequency. This term may be replaced with chemical shift.

Page 93: Fig. 3.48: The second gradient should be shown with opposite sign to the first, thus:

Page 123: Structure 4.3: A square bracket to the left of the compound is missing.

Page 138: INEPT signal intensities: First line should be "CH: I µsin q"

Page 201: Section 5.7, line 6: "...spectra based scalar couplings" should read "spectra based on scalar couplings"

Page 286: 13th/14th line from bottom: "... NOE as a function tc" should read "...NOE as a function of tc"

Page 290: Fig. 8.11: symbol p1* should read pI*, thus:

 

Page 369: Above "The PFG stimulated-echo" section: The text "G2/T2m-2" should not be there,- it is in fact the axis label for Fig. 9.36 on the following page.