Issue 3, 2016

Kinetics analysis and automated online screening of aminocarbonylation of aryl halides in flow

Abstract

Temperature, pressure, gas stoichiometry, and residence time were varied to control the yield and product distribution of the palladium-catalyzed aminocarbonylation of aromatic bromides in both a silicon microreactor and a packed-bed tubular reactor. Automation of the system set points and product sampling enabled facile and repeatable reaction analysis with minimal operator supervision. It was observed that the reaction was divided into two temperature regimes. An automated system was used to screen steady-state conditions for offline analysis by gas chromatography to fit a reaction rate model. Additionally, a transient temperature ramp method utilizing online infrared analysis was used, leading to more rapid determination of the reaction activation energy of the lower temperature regimes. The entire reaction spanning both regimes was modeled in good agreement with the experimental data.

Graphical abstract: Kinetics analysis and automated online screening of aminocarbonylation of aryl halides in flow

Supplementary files

Article information

Article type
Paper
Submitted
09 Jan 2016
Accepted
12 Feb 2016
First published
22 Feb 2016
This article is Open Access
Creative Commons BY license

React. Chem. Eng., 2016,1, 272-279

Kinetics analysis and automated online screening of aminocarbonylation of aryl halides in flow

J. S. Moore, C. D. Smith and K. F. Jensen, React. Chem. Eng., 2016, 1, 272 DOI: 10.1039/C6RE00007J

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