A continuous flow-batch hybrid reactor for commodity chemical synthesis enabled by inline NMR and temperature monitoring. Issue 38 (20th September 2018)

• Record Type: Journal Article
• Authors: Schotten, Christiane; Howard, Joseph L.; Jenkins, Robert L.; Codina, Anna; Browne, Duncan L.
• Is Part Of: Tetrahedron. Volume 74:Issue 38(2018)
• Page Start: 5503
• Page End: 5509
• Publication Date: 2018-09-20
• Subjects: Continuous flow -- Flow NMR -- Inline monitoring -- Exotherm control -- Space time yield; Chemistry, Organic -- Periodicals; 547.005
• DOI: 10.1016/j.tet.2018.05.070
• Languages: English
• ISSNs: 0040-4020

Abstract

Abstract: Inline, real time NMR and temperature measurements have been used to optimise the continuous flow synthesis of difluoromethyltrimethylsilane (TMSCF2 H) 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 TMSCF2 H after 105 min. Graphical abstract: Image 1