Issue 2, 2020

Online reaction monitoring by single-scan 2D NMR under flow conditions

Abstract

Nuclear magnetic resonance (NMR) spectroscopy is a powerful tool for reaction monitoring. Several devices have been recently developed for online monitoring, using flow NMR, of batch reactions carried out under realistic experimental conditions in terms of, e.g., agitation and temperature. Here we show that time series of single-scan ultrafast 2D NMR (UF2DNMR) spectra can be collected to monitor solution mixtures that circulate in a flow unit. Fast multidimensional NMR methods have the demonstrated potential to provide kinetic and mechanistic information on reactions. UF2DNMR makes it possible to collect 2D data sets in less than one second, but relies on spatial encoding (SPEN) that is sensitive to sample motion, thus making online monitoring challenging. We characterize the interference between flow and spatial encoding and provide pulse-sequence- and hardware-based solutions. The resulting method is illustrated with the monitoring of a saponification reaction. UF2DNMR with a flow unit is a promising tool for the online monitoring of organic chemical reactions.

Graphical abstract: Online reaction monitoring by single-scan 2D NMR under flow conditions

Supplementary files

Article information

Article type
Paper
Submitted
06 Sept. 2019
Accepted
11 Nov. 2019
First published
12 Nov. 2019

Analyst, 2020,145, 478-485

Online reaction monitoring by single-scan 2D NMR under flow conditions

C. Jacquemmoz, F. Giraud and J. Dumez, Analyst, 2020, 145, 478 DOI: 10.1039/C9AN01758E

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