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Efficient investigation of continuous reaction processes using gradients

Efficient investigation of continuous reaction processes using gradients
Efficient investigation of continuous reaction processes using gradients
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.
University of Southampton
Alston, Stephen
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Alston, Stephen
ebea2c1e-5552-4178-8b50-1a1e18903488
Whitby, Richard J.
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Alston, Stephen (2019) Efficient investigation of continuous reaction processes using gradients. University of Southampton, Doctoral Thesis, 271pp.

Record type: Thesis (Doctoral)

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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Published date: May 2019

Identifiers

Local EPrints ID: 451327
URI: http://eprints.soton.ac.uk/id/eprint/451327
PURE UUID: ceb08c4f-6a36-4314-9d8c-a678d6f1471b
ORCID for Stephen Alston: ORCID iD orcid.org/0000-0003-3829-0077
ORCID for Richard J. Whitby: ORCID iD orcid.org/0000-0002-9891-5502

Catalogue record

Date deposited: 21 Sep 2021 16:30
Last modified: 17 Mar 2024 02:32

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Contributors

Author: Stephen Alston ORCID iD
Thesis advisor: Richard J. Whitby ORCID iD

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