Breitmaier E. Structure elucidation by NMR in organic chemistry. A practical guide

3rd rev. ed. — Wiley, 2002. — XII, 258 p. — ISBN 0-470-85006-X; 0-470-85007-8.This text provides the graduate student with a systematic guide to unravelling structural information from the NMR spectra of unknown synthetic and natural compounds.
A brief introduction gives an overview of the basic principles and elementary instrumental methods of NMR. This is followed by instructional strategy and tactical advice on how to translate spectra into meaningful structural information. The book provides the student with 55 sets of spectra of graduated complexity. These are designed to challenge the student's problem-solving abilities by the introduction of new concepts with each group of problems, followed by possible solutions and full explanations. A formula index of solutions is provided at the end of the text.
This third edition, following on from the second (a reprint of the first edition with corrections), presents significant new material. Thus, actual methods of two-dimensional NMR such as some inverse techniques of heteronuclear shift correlation, as well as the detection of proton-proton connectivities and nuclear Overhauser effects are included. To demonstrate the applications of these methods, new problems have replaced those of previous editions.This book, based on many lectures and seminars, attempts to provide advanced undergraduates and graduate students with a systematic, readable and inexpensive introduction to the methods of structure determination by NMR. Chapter 1 starts with a deliberately concise survey of the basic terms, parameters and techniques dealt with in detail in other books, which cover the basic principles of NMR, pulse sequences as well as theoretical aspects of chemical shifts and spin-spin coupling, and which this workbook is not intended to replace. An introduction to basic strategies and tactics of structure determination using one- and two-dimensional NMR methods then follows in Chapter 2. Here, the emphasis is always on how spectra and associated parameters can be used to identify structural fragments. This chapter presents those topics that are essential for the identification of compounds or for solving structures, including atom connectivities, relative configuration and conformation, intra- and intermolecular interactions and, in some cases, molecular dynamics. Following the principle of 'learning by doing', Chapter 3 presents a series of case studies, providing spectroscopic details of 55 compounds that illustrate typical applications of NMR techniques in the structural characterisation of both synthetic and natural products. The level of difficulty, the sophistication of the methodology required increases from question to question, so that all readers will be able to find material suited to their knowledge and ability. One can work independently, solve the problem from the spectra and check the result in the formula index, or follow the detailed solutions given in Chapter 4. The spectroscopic details are presented in a way that makes the maximum possible information available at a glance, requiring minimal page turning. Chemical shifts and coupling constants do not have to be read off from scales but are presented numerically, allowing the reader to concentrate directly on problem solving without the need for tedious routine work.
Actual methods of two dimensional NMR such as some inverse techniques of heteronuclear shift correlation experiments (HMQC, HSQC, HMBC), proton shift correlations (TOCSY) and two-dimensional detection of nuclear Overhauser effects (ROESY) are illustrated in Chapter 2 of this edition. New problems are added in Chapter 3 and 4 not only to replace some of the former ones but also in order to improve the quality and to demonstrate some applications of the actual methods shown in Chapter 2. All formulae have been redrawn using new software; all spectra have been scanned into the data file and the layout has been optimized. My thanks must go to Dr. Rudolf Hartmann for recording some of the two-dimensional NMR experiments, to Klaus Rotscheidt for scanning and his assistance in electronic editing, and especially to Julia Wade for having translated the original German text for the first English edition of this book.