Design, Validation, and Implementation of a Rapid-Injection NMR System
Design, Validation, and Implementation of a Rapid-Injection NMR System
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DOI：
10.1021/jo100837a
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发表时间：
2010-08-20
影响因子：
3.6
通讯作者：
Beutner, Gregory L.
中科院分区：
文献类型：
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作者：
Denmark, Scott E.;Williams, Bruce J.;Beutner, Gregory L.
设计和建造了快速注射核磁共振 (RINMR) 装置，可以通过核磁共振波谱实时观察快速化学反应。该仪器设计用于将计量体积的试剂快速（< 2 秒）注入并混合到旋转的 NMR 管中，然后快速采集化学过程演变产生的数据。该通用系统的各种设计标准包括能够在任何温度下输送任何化学试剂并允许观察任何原子核。记录了与该仪器的构造和实施相关的各种挑战，以及设备在体积和温度方面的准确性的验证。最后，以三个案例研究的形式展示了该技术的最终验证和可重复性，这些案例研究使用该仪器阐明了有机反应机制的各个方面。作者敦促感兴趣的各方不要开始构建自己的仪器，并邀请那些研究问题可能适合这种分析的人联系相应的作者以获取本文描述的装置。
A Rapid Injection NMR (RINMR) apparatus has been designed and constructed to allow the observation of fast chemical reactions in real time by NMR spectroscopy. The instrument was designed to allow the rapid (< 2 s) injection and mixing of a metered volume of a reagent into a spinning NMR tube followed by rapid acquisition of the data resulting from the evolution of the chemical process. The various design criteria for this universal system included the ability to deliver any chemical reagent at any temperature and allow for the observation of any nucleus. The various challenges associated with the construction and implementation of this instrument are documented along with the validation of the accuracy of the apparatus with respect to volume and temperature. Finally, the ultimate validation and reproducibility of the technique is presented in the form of three case studies that used the instrument to elucidate various aspects of organic reaction mechanisms. The authors urge interested parties to not embark on the construction of their own instrument and invite those whose research problems might be amenable to this kind of analysis to contact the corresponding author for access to the apparatus described herein.