Journal
PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY
Volume 129, Issue -, Pages 28-106Publisher
PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.pnmrs.2022.01.001
Keywords
NMR; Mechanism; Kinetics; Isotopes; In situ analysis; Titrations; Flow; Reaction monitoring; DOSY; Catalysis; Data processing; Equilibrium
Funding
- ERC [340163, 838616]
- SNSF [P2ZHP2181497]
- Syngenta
- University of Edinburgh
- China Scholarship Council
- University of Edinburgh School of Chemistry
- Criticat-EPSRC-CDT
- AstraZeneca
- GCL-J
- European Research Council (ERC) [838616, 340163] Funding Source: European Research Council (ERC)
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This tutorial-style review discusses the application of solution-phase NMR in analyzing the mechanisms of homogeneous organic and organometallic reactions and processes. It emphasizes the advantages of solution-phase NMR spectroscopy, such as non-destructive, quantitative analysis of various nuclei common to organic and organometallic reactions, providing detailed structural information. The review is divided into two parts: the first part introduces general techniques, equipment, and guidelines for their selection and application, while the second part presents case studies illustrating specific techniques and approaches.
A 'principles and practice' tutorial-style review of the application of solution-phase NMR in the analysis of the mechanisms of homogeneous organic and organometallic reactions and processes. This review of 345 references summarises why solution-phase NMR spectroscopy is uniquely effective in such studies, allowing non-destructive, quantitative analysis of a wide range of nuclei common to organic and organometallic reactions, providing exquisite structural detail, and using instrumentation that is routinely available in most chemistry research facilities. The review is in two parts. The first comprises an introduction to general techniques and equipment, and guidelines for their selection and application. Topics include practical aspects of the reaction itself, reaction monitoring techniques, NMR data acquisition and processing, analysis of temporal concentration data, NMR titrations, DOSY, and the use of isotopes. The second part comprises a series of 15 Case Studies, each selected to illustrate specific techniques and approaches discussed in the first part, including in situ NMR (H-1/2, B-10/11, C-13, N-15, F-19, Si-29, P-31), kinetic and equilibrium isotope effects, isotope entrainment, isotope shifts, isotopes at natural abundance, scalar coupling, kinetic analysis (VTNA, RPKA, simulation, steady-state), stopped-flow NMR, flow NMR, rapid injection NMR, pure shift NMR, dynamic nuclear polarisation, H-1/F-19 DOSY NMR, and in situ illumination NMR.(c) 2022 Elsevier B.V. All rights reserved.
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