Real-Time Reaction Monitoring with In Operando Flow NMR and FTIR Spectroscopy: Reaction Mechanism of Benzoxazole Synthesis
2021
Chae, Yeongseok | Min, Sein | Park, Eunjoon | Lim, Chaiho | Cheon, Cheol-Hong | Jeong, Keunhong | Kwak, Kyungwon | Cho, Minhaeng
In operando observation of reaction intermediates is crucial for unraveling reaction mechanisms. To address the sensitivity limitations of commercial ReactIR, a flow cell was integrated with a Fourier transform infrared (FTIR) spectrometer yielding a “flow FTIR” device coupled with an NMR spectrometer for the elucidation of reaction mechanisms. The former device detects the low-intensity IR peaks of reaction intermediates by adjusting the path length of the FTIR sample cell, whereas the flow NMR allows the quantitative analysis of reaction species, thus offsetting the limitations of IR spectroscopy resulting from different absorption coefficients of the normal modes. Using the flow NMR and FTIR device, the controversial mechanism of benzoxazole synthesis was conclusively determined by spectroscopic evaluation of the reaction intermediates. This system enabled the accurate acquisition of previously elusive kinetic data, such as the reaction time and rate-determining step. The implementation of reaction flow cells into NMR and FTIR systems could be widely applied to study various reaction mechanisms, including dangerous and harsh reactions, thus avoiding contact with potentially harmful reaction intermediates.
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