The assembly and use of continuous flow systems for chemical synthesis

Nature Protocols
Joshua Britton, Timothy F Jamison

Abstract

The adoption of and opportunities in continuous flow synthesis ('flow chemistry') have increased significantly over the past several years. Continuous flow systems provide improved reaction safety and accelerated reaction kinetics, and have synthesised several active pharmaceutical ingredients in automated reconfigurable systems. Although continuous flow platforms are commercially available, systems constructed 'in-lab' provide researchers with a flexible, versatile, and cost-effective alternative. Herein, we describe the assembly and use of a modular continuous flow apparatus from readily available and affordable parts in as little as 30 min. Once assembled, the synthesis of a sulfonamide by reacting 4-chlorobenzenesulfonyl chloride with dibenzylamine in a single reactor coil with an in-line quench is presented. This example reaction offers the opportunity to learn several important skills including reactor construction, charging of a back-pressure regulator, assembly of stainless-steel syringes, assembly of a continuous flow system with multiple junctions, and yield determination. From our extensive experience of single-step and multistep continuous flow synthesis, we also describe solutions to commonly encountered technical ...Continue Reading

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Citations

Jun 7, 2018·Angewandte Chemie·Niels WeidmannPaul Knochel
Jun 21, 2018·Chemical Society Reviews·Joshua BrittonGregory A Weiss
Mar 8, 2019·Chemical Society Reviews·Jianyong ZhangXiu-Ping Yan
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Oct 19, 2019·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Mafalda Dias Gomes, John M Woodley
Dec 15, 2019·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Saira MumtazMichael Oelgemöller
Oct 8, 2020·Angewandte Chemie·Johannes H HarenbergPaul Knochel
Nov 4, 2020·Chemical Society Reviews·Mara GuidiKerry Gilmore
Jun 18, 2021·Beilstein Journal of Organic Chemistry·Guido GambacortaIan R Baxendale
May 7, 2019·Chemical Reviews·Audrey BeillardFrédéric Lamaty
Oct 28, 2019·ACS Sustainable Chemistry & Engineering·Marc Escribà-GelonchVolker Hessel
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