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

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 exotherm...

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Bibliographic Details
Published inTetrahedron Vol. 74; no. 38; pp. 5503 - 5509
Main Authors Schotten, Christiane, Howard, Joseph L., Jenkins, Robert L., Codina, Anna, Browne, Duncan L.
Format Journal Article
LanguageEnglish
Published Elsevier Ltd 20.09.2018
Subjects
Continuous flow
Exotherm control
Flow NMR
Inline monitoring
Space time yield
Flow NMR
Space time yield
Exotherm control
Inline monitoring
Continuous flow
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Summary: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. [Display omitted]
ISSN:0040-4020
1464-5416
DOI:10.1016/j.tet.2018.05.070