Nantes Université, CNRS, CEISAM UMR 6230, 44000, Nantes, France.
Chemistry. 2022 Sep 16;28(52):e202201175. doi: 10.1002/chem.202201175. Epub 2022 Jul 28.
Online monitoring by flow NMR spectroscopy is a powerful approach to study chemical reactions and processes, which can provide mechanistic understanding, and drive optimisations. However, some of the most useful methods for mixture analysis and reaction monitoring are not directly applicable in flow conditions. This is the case of classic diffusion-ordered NMR spectroscopy (DOSY) methods, which can be used to separate the spectral information for mixture's components. We describe a fast and flow-compatible diffusion NMR experiment that makes it possible to collect accurate diffusion data for samples flowing at up to 3 mL/min. We use it to monitor the synthesis of a Schiff base with a flow-tube with a time resolution of approximately 2 minutes. The one-shot flow-compatible diffusion NMR described here open many avenues for reaction monitoring applications.
在线监测通过流核磁共振波谱学是一种强大的方法来研究化学反应和过程,可以提供机制理解,并推动优化。然而,一些最有用的混合物分析和反应监测方法在流动条件下并不直接适用。这就是经典的扩散有序核磁共振波谱(DOSY)方法的情况,它可用于分离混合物成分的光谱信息。我们描述了一种快速且与流动兼容的扩散 NMR 实验,可用于收集高达 3 mL/min 的流动样品的准确扩散数据。我们使用它来监测希夫碱的合成,使用流管的时间分辨率约为 2 分钟。这里描述的单次流动兼容扩散 NMR 为反应监测应用开辟了许多途径。