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时间分辨非均匀采样在反应监测中的优势:苄胺和丙烯酰胺的氮杂迈克尔加成反应的案例。

Benefits of time-resolved nonuniform sampling in reaction monitoring: The case of aza-Michael addition of benzylamine and acrylamide.

机构信息

Centre of New Technologies, University of Warsaw, Warsaw, Poland.

Faculty of Chemistry, University of Warsaw, Warsaw, Poland.

出版信息

Magn Reson Chem. 2021 Mar;59(3):213-220. doi: 10.1002/mrc.5105. Epub 2020 Oct 15.

DOI:10.1002/mrc.5105
PMID:33016346
Abstract

Monitoring of chemical reactions is best carried out using methods that sample the test object at a rate greater than the time scale of the processes taking place. The recently proposed time-resolved nonuniform sampling (TR-NUS) method allows the use of two-dimensional (2D) nuclear magnetic resonance (NMR) spectra for this purpose and provides a time resolution equivalent to that achievable using one-dimensional spectra. Herein, we show that TR-NUS acquired data eliminates 2D spectral line disturbances and enables more accurate signal integration and kinetics conclusions. The considerations are exemplified with a seemingly simple aza-Michael reaction of benzylamine and acrylamide. Surprisingly, the product identification is possible only using 2D spectra, although credible monitoring requires TR-NUS.

摘要

化学反应的监测最好采用取样速率大于发生过程时间尺度的方法进行。最近提出的时间分辨非均匀采样(TR-NUS)方法允许为此目的使用二维(2D)核磁共振(NMR)光谱,并提供相当于使用一维光谱可实现的时间分辨率。在这里,我们表明,TR-NUS 采集的数据消除了 2D 光谱线干扰,并能够更准确地进行信号积分和动力学结论。这些考虑因素通过苯甲胺和丙烯酰胺的看似简单的氮杂迈克尔反应得到了例证。令人惊讶的是,尽管需要 TR-NUS 进行可信监测,但仅使用 2D 光谱就可以进行产物鉴定。

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