Efficient investigation of continuous reaction processes using gradients

Abstract

Continuous chemistry has become a commonplace tool in laboratories in both academic and industry settings. The ease of automation and an accurate control over parameters have allowed continuous chemistry to excel in reaction optimisation and investigation as well as extraction of kinetic data. Additionally, several methods have been reported in the literature which utilise unique aspects of performing a reaction continuously such as varying the reaction time or temperature during an experiment.
Presented herein are two flow methodologies which utilise the generation of gradients to extract large amounts of data from a single experiment. The first is the switch-off method for the optimisation of irradiance time in a single flow photoreaction and is tested using a [2+2] photocyclisation reaction with both in-line and off-line data acquisition.
The second methodology is the concentration gradient methodology for extraction of reagent concentration data in a single experiment. The gradients are used in reagent concentration optimisation, ligand concentration optimisation, functional group compatibility scoping, and reaction troubleshooting.
A third methodology is presented which utilises multi-port valves to redirect the flow of a reagent plug repeatedly through an in-line detector to generate multiple time points in a single reaction. Several different setups are reported, and the methodology is combined with the concentration gradient method to generate both concentration and time data in a single experiment.

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Identifiers

ORCID for Stephen Alston: orcid.org/0000-0003-3829-0077

ORCID for Richard J. Whitby: orcid.org/0000-0002-9891-5502

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