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Automated generation of photochemical reaction data by transient flow experiments coupled with online HPLC analysis

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Abstract

The automated generation and acquisition of large-scale reaction data is crucial to recent progress in organic synthesis and pharmaceutical process development. To follow reaction progress over time, time-series of reaction data can be generated by transient flow experiments, which allow to investigate reactions in a short transient period between two steady-state operations of a continuous-flow microreactor. The acquisition of analytical data in this short transient period, however, remains challenging since separation techniques like HPLC – though able to cope with highly complex samples – are typically regarded as too slow for the required acquisition rates. We break the longstanding coupling between the timescale of the continuous-flow experiment and the acquisition rate of the analytical method with the introduction of the multiple heart-cutting interface, which allows for sample parking prior to sample analysis. Transient flow experiments are presented for the [2 + 2] cycloaddition between 1-methyl-2-quinolinone and coumarin. Competing homo- and crossdimerization reactions are quantitatively investigated in systematic reaction parameter screenings with more than 400 data points. Results provide precious insights into this complex photochemical system – not only for reaction optimization, but also for a more profound understanding of the involved chemical processes.

Graphical abstract: Automated generation of photochemical reaction data by transient flow experiments coupled with online HPLC analysis

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Supplementary files

Article information


Submitted
17 Feb 2020
Accepted
23 Mar 2020
First published
23 Mar 2020

React. Chem. Eng., 2020, Advance Article
Article type
Paper

Automated generation of photochemical reaction data by transient flow experiments coupled with online HPLC analysis

C. P. Haas, S. Biesenroth, S. Buckenmaier, T. van de Goor and U. Tallarek, React. Chem. Eng., 2020, Advance Article , DOI: 10.1039/D0RE00066C

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