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Issue 3, 2016
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Kinetics analysis and automated online screening of aminocarbonylation of aryl halides in flow

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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

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Publication details

The article was received on 09 Jan 2016, accepted on 12 Feb 2016 and first published on 22 Feb 2016


Article type: Paper
DOI: 10.1039/C6RE00007J
React. Chem. Eng., 2016,1, 272-279
  • Open access: Creative Commons BY license
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    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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