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Three step synthesis of benzylacetone and 4-(4-methoxyphenyl)butan-2-one in flow using micropacked bed reactors

Waldron, C; Cao, E; Cattaneo, S; Brett, GL; Miedziak, PJ; Wu, G; Sankar, M; ... Gavriilidis, A; + view all (2019) Three step synthesis of benzylacetone and 4-(4-methoxyphenyl)butan-2-one in flow using micropacked bed reactors. Chemical Engineering Journal , 377 , Article 119976. 10.1016/j.cej.2018.09.137. Green open access

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Abstract

The synthesis of benzylacetone from benzyl alcohol and of 4-(4-methoxyphenyl)butan-2-one from 4-methoxybenzyl alcohol, which were previously performed in a batch cascade, were successfully performed in a telescoped flow system consisting of three micropacked bed reactors and a tube-in-tube membrane to remove oxygen. The system consisted of approximately 10 mg of 1 wt% AuPd/TiO2 catalyst for oxidation, 150–250 mg of anatase TiO2 for C–C coupling and 10 mg of 1 wt% Pt/TiO2 for reduction, operating at 115 °C, 130 °C and 120 °C respectively. Oxygen and hydrogen flowrates were 2 and 1.5 NmL/min and alcohol solution inlet flowrates were 10–80 µL/min, while the system operated at a back pressure of 5 barg. This system achieved significantly increased yields of benzylacetone compared to the batch cascade (56% compared to 8%) and slightly increased yields of 4-(4-methoxyphenyl)butan-2-one (48% compared to 41% when using the same catalyst supports). The major advantage of the telescoped flow system was the ability to separate the three reactions, so that each reaction could have its own catalyst and operating conditions, which led to significant process intensification.

Type: Article
Title: Three step synthesis of benzylacetone and 4-(4-methoxyphenyl)butan-2-one in flow using micropacked bed reactors
Open access status: An open access version is available from UCL Discovery
DOI: 10.1016/j.cej.2018.09.137
Publisher version: https://doi.org/10.1016/j.cej.2018.09.137
Language: English
Additional information: This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Keywords: Telescoped synthesis, Cascade synthesis, Catalytic microreactor, Oxidation, Hydrogenation, Coupling
UCL classification: UCL
UCL > Provost and Vice Provost Offices > UCL BEAMS
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of Engineering Science
UCL > Provost and Vice Provost Offices > UCL BEAMS > Faculty of Engineering Science > Dept of Chemical Engineering
URI: https://discovery.ucl.ac.uk/id/eprint/10061067
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