Online quantitative mass spectrometry for the rapid adaptive optimisation of automated flow reactors

Holmes, Nicholas; Akien, Geoffrey R.; Savage, Robert J.D.; Stanetty, Christian; Baxendale, Ian R.; Blacker, A. John; Taylor, Brian A.; Woodward, Robert L.; Meadowse, Rebecca E.; Bourne, Richard A.

doi:10.1039/c5re00083a

Online quantitative mass spectrometry for the rapid adaptive optimisation of automated flow reactors

Holmes, Nicholas; Akien, Geoffrey R.; Savage, Robert J.D.; Stanetty, Christian; Baxendale, Ian R.; Blacker, A. John; Taylor, Brian A.; Woodward, Robert L.; Meadowse, Rebecca E.; Bourne, Richard A.

Authors

Nicholas Holmes

Geoffrey R. Akien

Robert J.D. Savage

Christian Stanetty

Professor Ian Baxendale i.r.baxendale@durham.ac.uk
Professor

A. John Blacker

Brian A. Taylor

Robert L. Woodward

Rebecca E. Meadowse

Richard A. Bourne

Abstract

An automated continuous reactor for the synthesis of organic compounds, which uses online mass spectrometry (MS) for reaction monitoring and product quantification, is presented. Quantitative and rapid MS monitoring was developed and calibrated using HPLC. The amidation of methyl nicotinate with aqueous MeNH2 was optimised using design of experiments and a self-optimisation algorithm approach to produce >93% yield.

Citation

Holmes, N., Akien, G. R., Savage, R. J., Stanetty, C., Baxendale, I. R., Blacker, A. J., …Bourne, R. A. (2016). Online quantitative mass spectrometry for the rapid adaptive optimisation of automated flow reactors. Reaction Chemistry and Engineering, 1(1), 96-100. https://doi.org/10.1039/c5re00083a

Journal Article Type	Article
Acceptance Date	Nov 26, 2015
Online Publication Date	Dec 1, 2015
Publication Date	Feb 1, 2016
Deposit Date	Nov 26, 2015
Publicly Available Date	Nov 25, 2016
Journal	Reaction Chemistry and Engineering
Publisher	Royal Society of Chemistry
Peer Reviewed	Peer Reviewed
Volume	1
Issue	1
Pages	96-100
DOI	https://doi.org/10.1039/c5re00083a