In-Line Liquid-Liquid Separation for Laboratory-Scale Continuous-Flow Synthesis

One of the key benefits of flow chemistry is amenability to automation.  The Ley group has been a major proponent of using flow chemistry to simplify downstream processing by automating work-up procedures following flow reactions.  In addition to developing solid-supporting reagents and scavengers and monoliths for this purpose, we have developed technologies for the automated mechanical separation of liquid phases.

In 2007, our research group reported the first use of the Syrris FLLEX liquid-liquid membrane-based extraction unit to automate the workup of alcohol alkylations as a proof-of-principle demonstration [1].

In 2012, we reported the development of a prototype camera-and-computer based gravity separation unit [2].

Shortly afterwards, we advanced this technology for multiple in-line liquid-liquid separations in series, allowing workups to be automated over >24 h periods on reactions of >20 g scales. (D.X. Hu, M. O’Brien, S.V. Ley).

For a video demonstration of this technology, see click here.

Publications

1. A microcapillary flow disc (MFD) reactor for organic synthesis, C.H. Hornung, M.R. Mackley, I.R. Baxendale and S.V. Ley and, Org. Proc. Res. Dev2007, 11, 399-405.

2. A prototype continuous-flow liquid–liquid extraction system using open-source technology M. O’Brien, P. Koos, D.L. Browne, S.V. Ley, Org. Biomol. Chem. 2012,  10, 7031-7036.

3. Continuous multiple liquid–liquid separation: diazotization of amino acids in flow D.X. Hu , M. O’Brien, S.V. Ley, Org. Lett201214, 4246-4249.