Monitoring organic reactions by UF‐NMR spectroscopy

Abstract

a Standard 2D NMR experiments suffer from the many t 1 increments needed for spectra with sufficient digital resolution in the indirect dimension. Despite the different methodological approaches to overcome this problem, these increments have prevented studies of fast reactions. The development of ultrafast NMR (UF-NMR) has decisively speeded up the time scale of standard NMR to allow the study of organic reactions as they happen in real time to reveal mechanistic details. This mini-review summarizes the results achieved in monitoring organic reactions through this exciting technique.

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

“…The relevance of UF2DNMR for reaction monitoring has been demonstrated for reactions carried out in an NMR tube, with the detection or assignment of intermediates that could not be identified in 1D NMR monitoring, and with the measurement of their half-lives. 42,43 The possibility to collect reliable UF2DNMR data with a flow unit should thus provide this information in conditions that more closely replicate the reaction conditions of interest. While the analysis of more complex reactions is planned in our laboratory, it will require the installation of a ductless fume hood close to the NMR magnet.…”

“…[39][40][41] It is based on spatial parallelization of the indirect time dimension of 2D experiments, and makes it possible to obtain spectra in a single scan. The usefulness of UF2DNMR for reaction monitoring has been illustrated with mechanistic studies of organic chemical [42][43][44][45][46][47] and electrochemical reactions, 48 carried out in an NMR tube. It has also been used as an online detector in combination with a chromatography column and an HPLC system, 49,50 with no chemical reaction.…”

Ultrafast Maximum‐Quantum NMR Spectroscopy for the Analysis of Aromatic Mixtures

“…UF2D NMR has been shown to be useful to monitor chemical reaction at short reaction time and with increased time resolution . UF MQ NMR could complement the set of available UF pulse sequences, especially for aromatic compounds.…”

Insights into real-time chemical processes in a calcium sensor protein-directed dynamic library

“…NMR spectroscopy has been reported as a particularly useful technique to analyze protein–ligand interactions (e.g., STD-NMR, tr-NOESY) and to understand reaction mechanisms using Ultrafast NMR (UF-NMR) 23,24 .…”