4.4 Article

A continuous flow-batch hybrid reactor for commodity chemical synthesis enabled by inline NMR and temperature monitoring

Journal

TETRAHEDRON
Volume 74, Issue 38, Pages 5503-5509

Publisher

PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.tet.2018.05.070

Keywords

Continuous flow; Flow NMR; Inline monitoring; Exotherm control; Space time yield

Funding

  1. School of Chemistry at Cardiff University
  2. Cambridge Reactor Design

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Inline, real time NMR and temperature measurements have been used to optimise the continuous flow synthesis of difluoromethyltrimethylsilane (TMSCF2H) by the reduction of the Ruppert-Prakash reagent (TMSCF3). These measurements were used to maximise the space-time-yield, while ensuring this exothermic process remains safe. In this way, a three-fold increase in space-time-yield was achieved compared to the reported batch procedure, isolating 25 g of pure TMSCF2H after 105 min. (C) 2018 Published by Elsevier Ltd.

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