Quantitative and convenient real-time reaction monitoring using stopped-flow benchtop NMR

Abstract

Nuclear magnetic resonance (NMR) spectroscopy has the potential to serve as a widely applied reaction monitoring tool, particularly provided the growth in commercially available benchtop NMR systems and accompanying flow...

Low-Field Flow 31P NMR Spectroscopy for Organometallic Chemistry: On-Line Analysis of Highly Air-Sensitive Rhodium Diphosphine Complexes

“…All benchtop NMR instruments can be used for 1 H and 19 F analysis. 13 C and (multinuclear) heteroatom analysis requires a (tunable) dual-channel probe, for which much less NMR systems are available at present.…”

“…Applications in flow environments are still rather limited; however, first case studies of incorporation into flow chemistry and lab automation have been described and show the potential of this approach . It should furthermore be noted that reports on the use of heteroatom LF NMR are very limited. , Significantly lower spectral resolution can be obtained in LF 1 H NMR under standard operating conditions due to the low frequency of the spectrometers. Additionally, signal overlap may arise and complicate the correct interpretation of the spectrum, especially in cases where scalar couplings decrease the signal-to-noise ratio (SNR).…”

“…11 It should furthermore be noted that reports on the use of heteroatom LF NMR are very limited. 12,13 Significantly lower spectral resolution can be obtained in LF 1 H NMR under standard operating conditions due to the low frequency of the spectrometers. Additionally, signal overlap may arise and complicate the correct interpretation of the spectrum, especially in cases where scalar couplings decrease the signal-to-noise ratio (SNR).…”

Continuous flow synthesis of pyridinium salts accelerated by multi-objective Bayesian optimization with active learning

“…and purications or separations coupled with automation enhances the utility of ow techniques for high-throughput and autonomous experimentation. [24][25][26][27][28][29][30][31] Recently, there have been tremendous strides made towards fully autonomous (closed-loop) experimentation systems that require little to no human intervention once initiated, and undoubtedly these systems will continue to mature and nd value in research labs. 16,[32][33][34] In contrast to fully self-driving labs, there are many opportunities for human-in-the-loop and interactive ML to make an impact.…”

From at-line to online NMR: coupling probe-based autosampler with benchtop NMR

“…6 To address these quantification challenges, Jason Hein et al reported an innovative approach that utilizes a stopped-flow NMR system. 7 This method employs a Python script to facilitate the efficient transfer of the analyte to the spectrometer at predetermined time intervals. By conducting the data acquisition under static, no-flow conditions, quantitative complications associated with continuous flow are eliminated, resulting in a more straightforward and reliable analysis.…”