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Mechanistic analysis by NMR spectroscopy: A users guide
Progress in Nuclear Magnetic Resonance Spectroscopy ( IF 6.1 ) Pub Date : 2022-01-19 , DOI: 10.1016/j.pnmrs.2022.01.001
Yael Ben-Tal 1 , Patrick J Boaler 1 , Harvey J A Dale 1 , Ruth E Dooley 2 , Nicole A Fohn 1 , Yuan Gao 1 , Andrés García-Domínguez 1 , Katie M Grant 1 , Andrew M R Hall 1 , Hannah L D Hayes 1 , Maciej M Kucharski 1 , Ran Wei 1 , Guy C Lloyd-Jones 1
Affiliation  

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 (1/2H, 10/11B, 13C, 15N, 19F, 29Si, 31P), 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, 1H/19F DOSY NMR, and in situ illumination NMR.



中文翻译:

通过 NMR 光谱进行机械分析:用户指南

对液相核磁共振在均相有机和有机金属反应和过程机理分析中应用的“原理与实践”教程式回顾。这篇对 345 篇参考文献的综述总结了为什么溶液相 NMR 光谱在此类研究中具有独特的有效性,允许对有机和有机金属反应中常见的各种原子核进行非破坏性定量分析,提供精致的结构细节,并使用常规仪器可在大多数化学研究设施中使用。审查分为两部分。第一部分包括对一般技术和设备的介绍,以及它们的选择和应用指南。主题包括反应本身的实际方面、反应监测技术、NMR 数据采集和处理、分析时间浓度数据、NMR 滴定、DOSY 和同位素的使用。第二部分包括一系列 15 个案例研究,每个案例研究都是为了说明第一部分中讨论的具体技术和方法,包括原位NMR(1/2 H、10/11 B、13 C、15 N、19 F、29 Si、31 P)、动力学和平衡同位素效应、同位素夹带、同位素位移、天然丰度同位素、标量耦合、动力学分析(VTNA、RPKA、模拟、稳态)、停流 NMR、流动 NMR、快速注入 NMR、纯位移 NMR、动态核极化、1 H/ 19 F DOSY NMR 和原位照明 NMR。

更新日期:2022-01-19
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