Chemistry: A European Journal 2014-01-03

Investigation of a lithium-halogen exchange flow process for the preparation of boronates by using a cryo-flow reactor.

James A Newby, Lena Huck, D Wayne Blaylock, Paul M Witt, Steven V Ley, Duncan L Browne

Index: Chemistry 20(1) , 263-71, (2014)

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Abstract

Conducting low-temperature organometallic reactions under continuous flow conditions offers the potential to more accurately control exotherms and thus provide more reproducible and scalable processes. Herein, progress towards this goal with regards to the lithium-halogen exchange/borylation reaction is reported. In addition to improving the scope of substrates available on a research scale, methods to improve reaction profiles and expedite purification of the products are also described. On moving to a continuous system, thermocouple measurements have been used to track exotherms and provide a level of safety for continuous processing of organometallic reagents. The use of an in-line continuous liquid-liquid separation device to circumvent labour intensive downstream off-line processing is also reported. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.