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E-raamat: Essential Practical NMR for Organic Chemistry [Wiley Online]

(GlaxoSmithKline R&D Ltd), (GlaxoSmithKline R&D Ltd)
  • Formaat: 232 pages
  • Ilmumisaeg: 10-Dec-2010
  • Kirjastus: John Wiley & Sons Inc
  • ISBN-10: 470976403
  • ISBN-13: 9780470976401
Teised raamatud teemal:
  • Wiley Online
  • Hind: 95,16 €*
  • * hind, mis tagab piiramatu üheaegsete kasutajate arvuga ligipääsu piiramatuks ajaks
Essential Practical NMR for Organic ChemistrySuurem pilt
  • Formaat: 232 pages
  • Ilmumisaeg: 10-Dec-2010
  • Kirjastus: John Wiley & Sons Inc
  • ISBN-10: 470976403
  • ISBN-13: 9780470976401
Teised raamatud teemal:
Wiley Online e-raamatudRohkem infot Wiley Online kohta
Raamatu kodulehekülg: https://onlinelibrary.wiley.com/doi/book/10.1002/9780470976401
This book describes the use of NMR spectroscopy for dealing with problems of small organic molecule structural elucidation. It features a significant amount of vital chemical shift and coupling information but more importantly, it presents sound principles for the selection of the techniques relevant to the solving of particular types of problem, whilst stressing the importance of extracting the maximum available information from the simple 1-D proton experiment and of using this to plan subsequent experiments. Proton NMR is covered in detail, with a description of the fundamentals of the technique, the instrumentation and the data that it provides before going on to discuss optimal solvent selection and sample preparation. This is followed by a detailed study of each of the important classes of protons, breaking the spectrum up into regions (exchangeables, aromatics, heterocyclics, alkenes etc.). This is followed by consideration of the phenomena that we know can leave chemists struggling; chiral centres, restricted rotation, anisotropy, accidental equivalence, non-first-order spectra etc.  Having explained the potential pitfalls that await the unwary, the book then goes on to devote chapters to the chemical techniques and the most useful instrumental ones that can be employed to combat them.

A discussion is then presented on carbon-13 NMR, detailing its pros and cons and showing how it can be used in conjunction with proton NMR via the pivotal 2-D techniques (HSQC and HMBC) to yield vital structural information. Some of the more specialist techniques available are then discussed, i.e. flow NMR, solvent suppression, Magic Angle Spinning, etc. Other important nuclei are then discussed and useful data supplied. This is followed by a discussion of the neglected use of NMR as a tool for quantification and new techniques for this explained. The book then considers the safety aspects of NMR spectroscopy, reviewing NMR software for spectral prediction and data handling and concludes with a set of worked Q&As.

Introduction xi
1 Getting Started
1(10)
1.1 The Technique
1(1)
1.2 Instrumentation
2(1)
1.3 CW Systems
2(1)
1.4 FT Systems
3(8)
1.4.1 Origin of the Chemical Shift
6(1)
1.4.2 Origin of `Splitting'
7(2)
1.4.3 Integration
9(2)
2 Preparing the Sample
11(12)
2.1 How Much Sample Do I Need?
12(1)
2.2 Solvent Selection
13(4)
2.2.1 Deutero Chloroform (CDC13)
14(1)
2.2.2 Deutero Dimethyl Sulfoxide (D6-DMSO)
14(1)
2.2.3 Deutero Methanol (CD3OD)
15(1)
2.2.4 Deutero Water (D2O)
16(1)
2.2.5 Deutero Benzene (C6D6)
16(1)
2.2.6 Carbon Tetrachloride (CCl4)
16(1)
2.2.7 Trifluoroacetic Acid (CF3COOH)
16(1)
2.2.8 Using Mixed Solvents
17(1)
2.3 Spectrum Referencing (Proton NMR)
17(1)
2.4 Sample Preparation
18(5)
2.4.1 Filtration
19(4)
3 Spectrum Acquisition
23(10)
3.1 Number of Transients
23(1)
3.2 Number of Points
24(1)
3.3 Spectral Width
25(1)
3.4 Acquisition Time
25(1)
3.5 Pulse Width/Pulse Angle
25(2)
3.6 Relaxation Delay
27(1)
3.7 Number of Increments
27(1)
3.8 Shimming
28(2)
3.9 Tuning and Matching
30(1)
3.10 Frequency Lock
30(1)
3.10.1 Run Unlocked
30(1)
3.10.2 Internal Lock
30(1)
3.10.3 External Lock
31(1)
3.11 To Spin or Not to Spin?
31(2)
4 Processing
33(8)
4.1 Introduction
33(1)
4.2 Zero Filling and Linear Prediction
33(1)
4.3 Apodization
34(2)
4.4 Fourier Transformation
36(1)
4.5 Phase Correction
36(2)
4.6 Baseline Correction
38(1)
4.7 Integration
39(1)
4.8 Referencing
39(1)
4.9 Peak Picking
39(2)
5 Interpreting Your Spectrum
41(26)
5.1 Common Solvents and Impurities
44(2)
5.2 Group 1 - Exchangeables and Aldehydes
46(2)
5.3 Group 2 - Aromatic and Heterocyclic Protons
48(13)
5.3.1 Monosubstituted Benzene Rings
50(4)
5.3.2 Multisubstituted Benzene Rings
54(3)
5.3.3 Heterocyclic Ring Systems (Unsaturated) and Polycyclic Aromatic Systems
57(4)
5.4 Group 3 - Double and Triple Bonds
61(2)
5.5 Group 4 - Alkyl Protons
63(4)
6 Delving Deeper
67(34)
6.1 Chiral Centres
67(5)
6.2 Enantiotopic and Diastereotopic Protons
72(2)
6.3 Molecular Anisotropy
74(2)
6.4 Accidental Equivalence
76(2)
6.5 Restricted Rotation
78(4)
6.6 Heteronuclear Coupling
82(19)
6.6.1 Coupling between Protons and 13C
82(2)
6.6.2 Coupling between Protons and 19F
84(3)
6.6.3 Coupling between Protons and 31P
87(2)
6.6.4 Coupling between 1H and other Heteroatoms
89(2)
6.6.5 Cyclic Compounds and the Karplus Curve
91(5)
6.6.6 Salts, Free Bases and Zwitterions
96(5)
7 Further Elucidation Techniques - Part 1
101(10)
7.1 Chemical Techniques
101(1)
7.2 Deuteration
101(2)
7.3 Basification and Acidification
103(1)
7.4 Changing Solvents
104(1)
7.5 Trifluoroacetylation
104(2)
7.6 Lanthanide Shift Reagents
106(1)
7.7 Chiral Resolving Agents
106(5)
8 Further Elucidation Techniques - Part 2
111(16)
8.1 Instrumental Techniques
111(1)
8.2 Spin Decoupling (Homonuclear, 1-D)
111(1)
8.3 Correlated Spectroscopy (2-D)
112(4)
8.4 Total Con-elation Spectroscopy (1- and 2-D)
116(1)
8.5 The Nuclear Overhauser Effect and Associated Techniques
116(11)
9 Carbon-13 NMR Spectroscopy
127(16)
9.1 General Principles and 1-D 13C
127(3)
9.2 2-D Proton-Carbon (Single Bond) Correlated Spectroscopy
130(3)
9.3 2-D Proton-Carbon (Multiple Bond) Correlated Spectroscopy
133(3)
9.4 Piecing It All Together
136(1)
9.5 Choosing the Right Tool
137(6)
10 Some of the Other Tools
143(8)
10.1 Linking HPLC with NMR
143(1)
10.2 Flow NMR
144(1)
10.3 Solvent Suppression
145(1)
10.4 Magic Angle Spinning NMR
146(1)
10.5 Other 2-D Techniques
147(2)
10.5.1 Inadequate
147(1)
10.5.2 J-Resolved
147(1)
10.5.3 Diffusion Ordered Spectroscopy
148(1)
10.6 3-D Techniques
149(2)
11 Some of the Other Nuclei
151(6)
11.1 Fluorine
151(1)
11.2 Phosphorus
152(1)
11.3 Nitrogen
152(5)
12 Quantification
157(6)
12.1 Introduction
157(1)
12.2 Relative Quantification
157(1)
12.3 Absolute Quantification
158(2)
12.3.1 Internal Standards
158(1)
12.3.2 External Standards
158(1)
12.3.3 Electronic Reference
159(1)
12.3.4 Quantas Technique
159(1)
12.4 Things to Watch Out For
160(1)
12.5 Conclusion
161(2)
13 Safety
163(4)
13.1 Magnetic Fields
163(2)
13.2 Cryogens
165(1)
13.3 Sample-Related Injuries
166(1)
14 Software
167(6)
14.1 Acquisition Software
167(1)
14.2 Processing Software
167(2)
14.3 Prediction and Simulation Software
169(4)
14.3.1 13C Prediction
169(2)
14.3.2 1H Prediction
171(1)
14.3.3 Simulation
172(1)
14.3.4 Structural Verification Software
172(1)
14.3.5 Structural Elucidation Software
172(1)
15 Problems
173(32)
15.1 Ten NMR Problems
173(21)
15.2 Hints
194(1)
15.3 Answers
195(10)
Glossary 205(6)
Index 211
Steve Richards graduated in Chemistry from Bangor University in 1977 and completed an MSc in Analytical Chemistry at Bristol in 1979. He joined Glaxo Group Research in 1980 and has worked in the NMR spectroscopy department ever since. He has run regular courses in NMR interpretation for new graduates and sandwich students within GSK since the late 80s. John Hollerton joined the GSK spectroscopy department in 1980. Having spent time working with other spectroscopic techniques, he has been focused on NMR spectroscopy since 1982. He is now the manager with a staff of thirteen scientists working under his direction. John has also lectured internationally on the subject on many occasions.
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