Broadband ultrafast 2D NMR spectroscopy for online monitoring in continuous flow. 2023

Célia Lhoste, and Margherita Bazzoni, and Justine Bonnet, and Aurélie Bernard, and François-Xavier Felpin, and Patrick Giraudeau, and Jean-Nicolas Dumez
Nantes Université, CNRS, CEISAM UMR6230, F-44000 Nantes, France. jean-nicolas.dumez@univ-nantes.fr.

Flow NMR is a powerful tool to monitor chemical reactions under realistic conditions. Here, we describe ultrafast (UF) 2D NMR schemes that make it possible to acquire broadband homonuclear 2D NMR spectra in 90 seconds or less for a continuously flowing sample. An interleaved acquisition strategy is used to address the spectral width limitation of UF 2D NMR. We show how, for a flowing sample, the use of a transverse axis for spatial encoding makes it possible to achieve the very high scan-to-scan stability required for interleaved acquisition. We also describe an optimised solvent suppression strategy that is effective for interleaved acquisition in continuous flow. These developments open the way to online monitoring with flow 2D NMR at high time resolution, as we illustrate with the monitoring of an organocatalysed condensation reaction.

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