Rahman One and Two Dimensional NMR Spectroscopy

1. Auflage 2013
ISBN: 978-1-4832-9071-3
Verlag: Elsevier Science & Techn.
Format: PDF
Kopierschutz: 1 - PDF Watermark

E-Book, Englisch, 599 Seiten, Web PDF

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.

Atta-ur-Rahman, FRS, D.Phil., TI, SI HI, NI, is a leading scientist and scholar in the field of organic chemistry from Pakistan, especially renowned for his research in the various areas relating to natural product chemistry. With over 909 publications in the field of his expertise including 116 books largely published by leading publishers in Europe and USA and 27 patents, he is also credited for reviving the higher education and research practices in Pakistan. Prof. Rahman was elected as Fellow of Royal Society (London) in July 2006 thereby becoming one of the 4 scientists from the Muslim world to have ever won this honor in the last 350 years when the Royal Society was established. He is also the only scientist from the Muslim world to have been conferred the UNESCO Science Prize in 1999.[11] He has been conferred honorary doctorate degrees by many universities including the degree of Doctor of Science (Sc.D.) by Cambridge University (UK) (1987) and an Honorary degree of Doctor of Education by Coventry University UK in November 2007. He was elected Honorary Life Fellow of Kings College, Cambridge University, UK in 2007. Prof. Atta-ur-Rahman was conferred the TWAS Prize for Institution Building in Durban, South Africa in October 2009 in recognition of his contributions for bringing about revolutionary changes in the higher education sector in Pakistan. He was awarded the Engro Excellence Award in Science & Technology 2011 for meritorious contributions. He is President of Network of Academies of Sciences of Islamic Countries (NASIC) and the Vice-President (Central & South Asia) of the Academy of Sciences for the Developing World (TWAS) Council, and Foreign Fellow of Korean Academy of Sciences. Prof. Atta-ur-Rahman was the President of the Pakistan Academy of Sciences (2003-06), and was again elected President of Pakistan Academy of Sciences in January 2011. He was the Federal Minister for Science and Technology (14 March 2000 - 20 November 2002), Federal Minister of Education (2002) and Chairman of the Higher Education Commission with the status of a Federal Minister from 2002-2008. The Austrian government also honoured him with its highest civil award ('Das Große Goldene Ehrenzeichen am Bande', 2007) in recognition of his eminent contributions. Prof. Atta-ur-Rahman was the Coordinator General of COMSTECH, an OIC Ministerial Committee comprising the 57 Ministers of Science & Technology from 57 OIC member countries during 1996-2012. He is also the Patron of International Centre of Chemical and Biological Sciences (which comprises a number of institutes, including the Hussain Ebrahim Jamal Research Institute of Chemistry and the Dr. Panjwani Center of Molecular Medicine and Drug Development) at Karachi University. He established a research center on Genomics in Karachi University. In recognition of the eminent contributions of Prof. Atta-ur-Rahman, a number of institutions have been named after him within and outside Pakistan. These include a natural product chemistry institute (Atta-ur-Rahman Research Institute of Natural Product Discovery, RiND) at the University of Technology Mara in Malaysia, Atta-ur-Rahman School of Applied Biosciences at National University of Science & Technology in Islamabad, and Dr. Atta-ur-Rahman Building at the International Centre for Chemical and Biological Sciences, University of Karachi. The Academy of Sciences in the Developing World (TWAS) based in Trieste, Italy has introduced a Dr. Atta-ur-Rahman Prize in Chemistry to a scientist from the developing world each year. The Prize carries a cash award of $ 5,000 and a Certificate.

Autoren/Hrsg.

Rahman, Atta-Ur

Inhaltsverzeichnis

1;Front Cover;1
2;One and Two Dimensional NMR Spectroscopy;4
3;Copyright Page;5
4;Table of Contents;10
5;PREFACE;6
6;FOREWORD;8
7;Chapter 1. Basic Principles of Modern NMR Spectroscopy;22
7.1;1.1 INTRODUCTION;22
7.2;1.2 SOME FUNDAMENTAL CONSIDERATIONS IN NMR SPECTROSCOPY;23
7.3;REFERENCES;93
8;Chapter 2. Spin-Echo and Polarisation Transfer;98
8.1;2.1 SPIN-ECHO FORMATION IN HOMONUCLEAR AND HETERONUCLEAR SYSTEMS;98
8.2;2.2 CROSS-POLARISATION;115
8.3;2.3. PROBLEMS;146
8.4;2.4 SOLUTIONS TO PROBLEMS IN APT, INEPT AND DEPT;154
8.5;REFERENCES;159
9;Chapter 3. Carbon-Carbon Connectivity-1D-INADEQUATE Spectra;162
9.1;3.1 INTRODUCTION;162
9.2;3.2 ONE-DIMENSIONAL INADEQUATE 13C-NMR SPECTRA;164
9.3;REFERENCES;185
10;Chapter 4.
The Nuclear Overhauser Effect;188
10.1;4.1 INTRODUCTION;188
10.2;4.2 RELAXATION PATHWAYS;189
10.3;4.3 HOW NOE OCCURS;190
10.4;4.4 OTHER FACTORS GOVERNING RELAXATION AND NOE;195
10.5;4.5 INTERNUCLEAR DISTANCE AND NOE;199
10.6;4.6 HETERONUCLEAR NOE;205
10.7;4.7 NOE DIFFERENCE SPECTRA;206
10.8;4.8 PROBLEMS IN NOE DIFFERENCE SPECTROSCOPY;215
10.9;4.9 SOLUTIONS TO NOE PROBLEMS;218
10.10;REFERENCES;221
11;Chapter 5. Two-Dimensional NMR Spectroscopy — Basic Principles;224
11.1;REFERENCES;236
12;Chapter 6. Heteronuclear 2D J-Resolved Spectroscopy;238
12.1;6.1 THE GATED DECOUPLER METHOD;243
12.2;6.2 THE REFOCUSSED FOLD-OVER CORRECTED (RE-FOCSY) GATED DECOUPLER METHOD;246
12.3;6.3 THE SPIN-FLIP METHOD;247
12.4;6.4 THE SELECTIVE SPIN-FLIP METHOD;247
12.5;6.5 THE SEMI-SELECTIVE SPIN-FLIP METHOD;251
12.6;6.6 INDIRECT J-SPECTROSCOPY WITH SELECTIVE SPIN-FLIP;255
12.7;6.7 HETERONUCLEAR 2D J-RESOLVED SPECTRA WITH POLARISATION TRANSFER;256
12.8;6.8 HETERONUCLEAR 2D J-RESOLVED SPECTRA WITH DRIVEN PULSES;257
12.9;6.9 PROBLEMS IN HETERONUCLEAR 2D J-RESOLVED SPECTROSCOPY;258
12.10;6.10 SOLUTIONS TO HETERONUCLEAR 2D J-RESOLVED SPECTRAL PROBLEMS;260
12.11;REFERENCES;263
13;Chapter 7. Homonuclear 2D J-Resolved Spectroscopy;266
13.1;7.1 DOUBLE RESONANCE IN 2D J-RESOLVED SPECTRA;276
13.2;7.2 CONSTANT TIME 2D J-RESOLVED SPECTRA;276
13.3;7.3 ABSORPTION MODE 2D J-RESOLVED SPECTRA;278
13.4;7.4 DIFFERENTIATION OF HOMONUCLEAR MULTIPLETS BY INDIRECT 2D J- RESOLVED SPECTROSCOPY;279
13.5;7.5 PROBLEMS IN 2D J-RESOLVED SPECTROSCOPY;281
13.6;7.6 SOLUTIONS TO 2D J-RESOLVED SPECTRAL PROBLEMS;285
13.7;REFERENCES;288
14;Chapter 8. Homonuclear 2D Shift Correlated Spectroscopy;290
14.1;8.1 COSY SPECTRA;290
14.2;8.2 MODIFICATIONS IN COSY SPECTRA;338
14.3;8.3 PROBLEMS IN COSY;370
14.4;8.4 SOLUTIONS TO PROBLEMS IN COSY;373
14.5;REFERENCES;376
15;Chapter 9. Chemical Shift Correlation Through Cross-Relaxation and Exchange;380
15.1;9.1 INTRODUCTION;380
15.2;9.2 NUCLEAR OVERHAUSER ENHANCEMENT SPECTROSCOPY (NOESY);381
15.3;9.3 2D CHEMICAL EXCHANGE SPECTRA;390
15.4;9.4 CAMELSPIN OR ROESY (ROTATING FRAME O_VERHAUSER E_NHANCEMENT SPECTROSCOPY_);394
15.5;9.5 TWO-DIMENSIONAL HETERONUCLEAR NOE SPECTROSCOPY (HOESY);397
15.6;9.6 COMBINED COSY-NOESY EXPERIMENT (COCONOSY);400
15.7;9.7 DQ NOESY;401
15.8;9.8 PROBLEMS IN NOESY;402
15.9;9.9 SOLUTIONS TO PROBLEMS IN NOESY;405
15.10;REFERENCES;408
16;Chapter 10. Heteronuclear 2D Shift Correlation Spectroscopy;412
16.1;10.1 PRINCIPLES OF HETERONUCLEAR 2D-SHIFT CORRELATION SPECTROSCOPY;412
16.2;10.2 MODIFICATIONS OF HETERONUCLEAR 2D-SHIFT CORRELATION EXPERIMENT;419
16.3;10.3 SENSITIVITY OF HETERONUCLEAR COHERENCE TRANSFER EXPERIMENTS;435
16.4;10.4 HETERONUCLEAR RELAYED COHERENCE TRANSFER SPECTROSCOPY (OR HETERONUCLEAR RELAYED COSY);437
16.5;10.5 PROBLEMS IN HETERO-COSY;448
16.6;10.6 SOLUTIONS TO HETERO-COSY PROBLEMS;450
16.7;REFERENCES;452
17;Chapter 11. Cross-Polarisation in the Rotating Frame;456
17.1;11.1 INTRODUCTION;456
17.2;11.2 HOMONUCLEAR HARTMANN-HAHN SPECTROSCOPY (HOHAHA);457
17.3;REFERENCES;465
18;Chapter 12. 2D Multiple-Quantum Spectroscopy;468
18.1;12.1 INTRODUCTION;468
18.2;12.2 MULTIPLE-QUANTUM SPECTRA OF TWO-SPIN SYSTEMS;471
18.3;12.3 MULTIPLE- QUANTUM SPECTRA OF THREE-SPIN SYSTEMS;480
18.4;12.4 MULTIPLE QUANTUM SPECTRA IN FOUR-SPIN SYSTEMS;488
18.5;12.5 UNIFORM EXCITATION OF MULTIPLE- QUANTUM COHERENCE;489
18.6;12.6 MULTIPLE- QUANTUM FILTERED COSY SPECTRA;491
18.7;12.7 H0MONUCLEAR ZERO-QUANTUM SPECTROSCOPY;496
18.8;12.8 PROBLEMS (2D-INADEQUATE);505
18.9;12.9 SOLUTIONS TO PROBLEMS (2D-INADEQUATE);508
18.10;REFERENCES;510
19;Chapter 13. Tackling the Structure;514
19.1;13.1 CHOICE OF EXPERIMENT;514
19.2;13.2 A CASE STUDY;516
19.3;REFERENCE;531
20;Chapter 14. Product Operators Approach to 2D-NMR Spectroscopy;532
20.1;14.1 SCALAR COUPLING;535
20.2;14.2 DIPOLAR COUPLING;539
20.3;14.3 PHASE CYCLING AND PRODUCT OPERATORS;542
20.4;REFERENCES;547
21;Appendix 1:
SOME TERMS, SYMBOLS AND ACRONYMS USED IN NMR SPECTROSCOPY;548
22;Appendix 2:
SUMMARY OF IMPORTANT 2D NMR TECHNIQUES;558
22.1;REFERENCES;565
23;INDEX;574