One and Two Dimensional NMR Spectroscopy (eBook)

Atta-ur- Rahman (Autor)

eBook Download: PDF

2013 | 1. Auflage
599 Seiten
Elsevier Science (Verlag)
978-1-4832-9071-3 (ISBN)

Infos

The field of nuclear magnetic resonance spectroscopy has undergone explosive development during the last decade with the advent of new one- and two-dimensional techniques. The author has had extensive experience in the use of these techniques for the structure elucidation of complex natural products, and in this book he gives a comprehensive, up-to-date and very readable account of these developments.

The book's scope is very wide. It starts from fundamental principles of modern NMR spectroscopy, describing the instrumentation and its optimum use, and extends to the latest developments such as inverse measurements. Emphasis is on problem-solving so as to be useful to a large number of organic chemists, biochemists and medicinal chemists. The problems and worked solutions at the end of the chapters will help students to gain proficiency in the application of these new techniques. Those who are learning how to operate modern NMR spectrometers will find particularly useful the description of such basic aspects as shimming, probe tuning, and methods for improvement of resolution and sensitivity.

Inhalt

Front Cover 1
One and Two Dimensional NMR Spectroscopy 4
Copyright Page 5
Table of Contents 10
PREFACE 6
FOREWORD 8
Chapter 1. Basic Principles of Modern NMR Spectroscopy 22
1.1 INTRODUCTION 22
1.2 SOME FUNDAMENTAL CONSIDERATIONS IN NMR SPECTROSCOPY 23
REFERENCES 93
Chapter 2. Spin-Echo and Polarisation Transfer 98
2.1 SPIN-ECHO FORMATION IN HOMONUCLEAR AND HETERONUCLEAR SYSTEMS 98
2.2 CROSS-POLARISATION 115
2.3. PROBLEMS 146
2.4 SOLUTIONS TO PROBLEMS IN APT, INEPT AND DEPT 154
REFERENCES 159
Chapter 3. Carbon-Carbon Connectivity-1D-INADEQUATE Spectra 162
3.1 INTRODUCTION 162
3.2 ONE-DIMENSIONAL INADEQUATE 13C-NMR SPECTRA 164
REFERENCES 185
Chapter 4. 
188 
4.1 INTRODUCTION 188
4.2 RELAXATION PATHWAYS 189
4.3 HOW NOE OCCURS 190
4.4 OTHER FACTORS GOVERNING RELAXATION AND NOE 195
4.5 INTERNUCLEAR DISTANCE AND NOE 199
4.6 HETERONUCLEAR NOE 205
4.7 NOE DIFFERENCE SPECTRA 206
4.8 PROBLEMS IN NOE DIFFERENCE SPECTROSCOPY 215
4.9 SOLUTIONS TO NOE PROBLEMS 218
REFERENCES 221
Chapter 5. Two-Dimensional NMR Spectroscopy — Basic Principles 224
REFERENCES 236
Chapter 6. Heteronuclear 2D J-Resolved Spectroscopy 238
6.1 THE GATED DECOUPLER METHOD 243
6.2 THE REFOCUSSED FOLD-OVER CORRECTED (RE-FOCSY) GATED DECOUPLER METHOD 246
6.3 THE SPIN-FLIP METHOD 247
6.4 THE SELECTIVE SPIN-FLIP METHOD 247
6.5 THE SEMI-SELECTIVE SPIN-FLIP METHOD 251
6.6 INDIRECT J-SPECTROSCOPY WITH SELECTIVE SPIN-FLIP 255
6.7 HETERONUCLEAR 2D J-RESOLVED SPECTRA WITH POLARISATION TRANSFER 256
6.8 HETERONUCLEAR 2D J-RESOLVED SPECTRA WITH DRIVEN PULSES 257
6.9 PROBLEMS IN HETERONUCLEAR 2D J-RESOLVED SPECTROSCOPY 258
6.10 SOLUTIONS TO HETERONUCLEAR 2D J-RESOLVED SPECTRAL PROBLEMS 260
REFERENCES 263
Chapter 7. Homonuclear 2D J-Resolved Spectroscopy 266
7.1 DOUBLE RESONANCE IN 2D J-RESOLVED SPECTRA 276
7.2 CONSTANT TIME 2D J-RESOLVED SPECTRA 276
7.3 ABSORPTION MODE 2D J-RESOLVED SPECTRA 278
7.4 DIFFERENTIATION OF HOMONUCLEAR MULTIPLETS BY INDIRECT 2D J- RESOLVED SPECTROSCOPY 279
7.5 PROBLEMS IN 2D J-RESOLVED SPECTROSCOPY 281
7.6 SOLUTIONS TO 2D J-RESOLVED SPECTRAL PROBLEMS 285
REFERENCES 288
Chapter 8. Homonuclear 2D Shift Correlated Spectroscopy 290
8.1 COSY SPECTRA 290
8.2 MODIFICATIONS IN COSY SPECTRA 338
8.3 PROBLEMS IN COSY 370
8.4 SOLUTIONS TO PROBLEMS IN COSY 373
REFERENCES 376
Chapter 9. Chemical Shift Correlation Through Cross-Relaxation and Exchange 380
9.1 INTRODUCTION 380
9.2 NUCLEAR OVERHAUSER ENHANCEMENT SPECTROSCOPY (NOESY) 381
9.3 2D CHEMICAL EXCHANGE SPECTRA 390
9.4 CAMELSPIN OR ROESY (ROTATING FRAME O_VERHAUSER E_NHANCEMENT SPECTROSCOPY_) 394
9.5 TWO-DIMENSIONAL HETERONUCLEAR NOE SPECTROSCOPY (HOESY) 397
9.6 COMBINED COSY-NOESY EXPERIMENT (COCONOSY) 400
9.7 DQ NOESY 401
9.8 PROBLEMS IN NOESY 402
9.9 SOLUTIONS TO PROBLEMS IN NOESY 405
REFERENCES 408
Chapter 10. Heteronuclear 2D Shift Correlation Spectroscopy 412
10.1 PRINCIPLES OF HETERONUCLEAR 2D-SHIFT CORRELATION SPECTROSCOPY 412
10.2 MODIFICATIONS OF HETERONUCLEAR 2D-SHIFT CORRELATION EXPERIMENT 419
10.3 SENSITIVITY OF HETERONUCLEAR COHERENCE TRANSFER EXPERIMENTS 435
10.4 HETERONUCLEAR RELAYED COHERENCE TRANSFER SPECTROSCOPY (OR HETERONUCLEAR RELAYED COSY) 437
10.5 PROBLEMS IN HETERO-COSY 448
10.6 SOLUTIONS TO HETERO-COSY PROBLEMS 450
REFERENCES 452
Chapter 11. Cross-Polarisation in the Rotating Frame 456
11.1 INTRODUCTION 456
11.2 HOMONUCLEAR HARTMANN-HAHN SPECTROSCOPY (HOHAHA) 457
REFERENCES 465
Chapter 12. 2D Multiple-Quantum Spectroscopy 468
12.1 INTRODUCTION 468
12.2 MULTIPLE-QUANTUM SPECTRA OF TWO-SPIN SYSTEMS 471
12.3 MULTIPLE- QUANTUM SPECTRA OF THREE-SPIN SYSTEMS 480
12.4 MULTIPLE QUANTUM SPECTRA IN FOUR-SPIN SYSTEMS 488
12.5 UNIFORM EXCITATION OF MULTIPLE- QUANTUM COHERENCE 489
12.6 MULTIPLE- QUANTUM FILTERED COSY SPECTRA 491
12.7 H0MONUCLEAR ZERO-QUANTUM SPECTROSCOPY 496
12.8 PROBLEMS (2D-INADEQUATE) 505
12.9 SOLUTIONS TO PROBLEMS (2D-INADEQUATE) 508
REFERENCES 510
Chapter 13. Tackling the Structure 514
13.1 CHOICE OF EXPERIMENT 514
13.2 A CASE STUDY 516
REFERENCE 531
Chapter 14. Product Operators Approach to 2D-NMR Spectroscopy 532
14.1 SCALAR COUPLING 535
14.2 DIPOLAR COUPLING 539
14.3 PHASE CYCLING AND PRODUCT OPERATORS 542
REFERENCES 547
Appendix 1: 
548 
Appendix 2: 
558 
REFERENCES 565
INDEX 574

Produkt-Details

• Erscheint lt. Verlag: 22.10.2013
• Sprache: englisch
• Themenwelt: Naturwissenschaften ► Chemie ► Analytische Chemie
• Themenwelt: Naturwissenschaften ► Physik / Astronomie ► Elektrodynamik
• Themenwelt: Technik
• ISBN-10: 1-4832-9071-9 / 1483290719
• ISBN-13: 978-1-4832-9071-3 / 9781483290713