Abstract
A new bespoke semi-continuous parallel column supercritical fluid chromatography unit has been developed that solves the problem of effective separation of continuous, multicomponent reaction mixtures.
Highlights
Isolating target products from multicomponent mixtures is a familiar challenge faced by chemists on a daily basis
In order to maintain the selectivity and broad usability offered by standard chromatography systems, we applied a semi-continuous mode of operation to columns arranged in parallel
Having prepared a quantity of crude reaction mixture, we identified suitable operating conditions for the separation as described in the Electronic supplementary information (ESI).† It was interesting to observe that product breakdown occurred when diethylaminopropyl polymer (DEAP) columns were used
Summary
Isolating target products from multicomponent mixtures is a familiar challenge faced by chemists on a daily basis. Techniques such as flash column chromatography, crystallisation and filtration are commonly employed to effect off-line purification. There are few such broadly versatile techniques to achieve the same outcome for continuous multi-step flow reactions. Commonly used separation techniques for continuous synthesis include liquid–liquid extraction,[2,3,4] filtration[5,6] and solid-supported scavenging and reagents.[7,8] While these can be extremely useful, when telescoping multiple reaction steps together,[9,10] where the output mixture from one reaction is linked directly with the input for the they are usually designed to remove individual impurities from mixtures, rather than isolating the compound of interest
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