Bolt, Robert RA;
Smallman, Harry R;
Leitch, Jamie A;
Bluck, Gavin W;
Barreteau, Fabien;
Iosub, Andrei V;
Constable, David;
... Browne, Duncan L; + view all
(2024)
Solvent Minimized Synthesis of Amides by Reactive Extrusion.
Angewandte Chemie International Edition
10.1002/anie.202408315.
(In press).
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Abstract
Herein, we report on the translation of a small scale ball-milled amidation protocol into a large scale continuous reactive extrusion process. Critical components to the successful translation were: a) understanding how the different operating parameters of a twin-screw extruder should be harnessed to control prolonged continuous operation, and b) consideration of the physical form of the input materials. The amidation reaction is applied to 36 amides spanning a variety of physical form combinations (liquid-liquid, solid–liquid and solid-solid). Following this learning process, we have developed an understanding for the translation of each physical form combination and demonstrated a 7-hour reactive extrusion process for the synthesis of an amide on 500 gram scale (1.3 mols of product).
| Type: | Article |
|---|---|
| Title: | Solvent Minimized Synthesis of Amides by Reactive Extrusion |
| Location: | Germany |
| Open access status: | An open access version is available from UCL Discovery |
| DOI: | 10.1002/anie.202408315 |
| Publisher version: | http://dx.doi.org/10.1002/anie.202408315 |
| Language: | English |
| Additional information: | © 2024 The Authors. Angewandte Chemie International Edition published by Wiley-VCH GmbH This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. |
| Keywords: | Science & Technology, Physical Sciences, Chemistry, Multidisciplinary, Chemistry, mechanochemistry, solvent-minimised, direct amidation, twin-screw extrusion, green chemistry, continuous flow, MECHANOCHEMICAL SYNTHESIS, ORGANIC-SYNTHESIS, PEPTIDE |
| UCL classification: | UCL UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Life Sciences UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Life Sciences > UCL School of Pharmacy UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Life Sciences > UCL School of Pharmacy > Pharmaceutics UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Life Sciences > UCL School of Pharmacy > Pharma and Bio Chemistry |
| URI: | https://discovery-pp.ucl.ac.uk/id/eprint/10197671 |
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