ABSTRACT
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.
ABSTRACT
This work demonstrates the in-line monitoring of a flow photochemical reaction using 1D and ultrafast 2D NMR methods at high magnetic field. The reaction mixture exiting the flow reactor is flown through the NMR spectrometer and directly analyzed. In the case of simple substrates, suitable information can be obtained through 1D 1 H spectra, but for molecules of higher complexity the use of 2D experiments is key to address signal overlaps and assignment issues. Here we show the usefulness of ultrafast 2D COSY experiments acquired in 70â s or less, for the in-line monitoring of photochemical reactions, and the possibility to obtain reliable quantitative information. This is a powerful framework to, for example, efficiently screen reaction conditions.