Fast Multidimensional Flow Nuclear Magnetic Resonance at High Field for Real‐Time Reaction Monitoring and Flow Synthesis

Flow nuclear magnetic resonance (NMR) at high field is regarded as a powerful technique for the online monitoring of chemical reactions, in which real-time quantitative and structural information is provided. Although 1D ¹H spectra are commonly acquired for such applications, the information content is often limited due to peak overlap and ambiguity in signal assignment. To address these limitations, 2D NMR methods are employed, allowing for the resolution of overlapping peaks and the acquisition of correlation information that facilitates assignment. Fast implementations of these 2D techniques have been developed, with durations ranging from sub-seconds to minutes, making them suitable for a wide range of online reaction monitoring applications. These methods are also expected to enhance flow synthesis applications, where flow reactors are hyphenated with high-field NMR spectrometers. In this context, a selection of fast 2D NMR methods compatible with flow NMR is presented, including ultrafast 2D NMR and fast diffusion-ordered NMR spectroscopy. Experimental setups and current best practices are outlined, and the principles behind each method, as well as their implementation for continuously flowing samples, are described. Flow-specific effects observed under different conditions are also discussed. These fast 2D NMR methods are anticipated to be of particular value to practitioners utilizing flow NMR for reaction monitoring.

• Bazzoni, M
• Horbenko, Y
• Sabbagh, N
• Marchand, A
• Grochowska‐Tatarczak, M
• Bernard, A
• Giraudeau, P
• Felpin, F
• Dumez, J

• Nantes Université CNRS UMR6230 CEISAM F‐44000 Nantes France

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