Using in situ Raman monitoring as a tool for rapid optimisation and scale-up of microwave-promoted organic synthesis: esterification as an example

Nicholas E Leadbeater; Rebecca J Smith; T Michael Barnard

doi:10.1039/b615597a

Using in situ Raman monitoring as a tool for rapid optimisation and scale-up of microwave-promoted organic synthesis: esterification as an example

Org Biomol Chem. 2007 Mar 7;5(5):822-5. doi: 10.1039/b615597a. Epub 2007 Jan 30.

Authors

Nicholas E Leadbeater¹, Rebecca J Smith, T Michael Barnard

Affiliation

¹ Department of Chemistry, University of Connecticut, 55 North Eagleville Road, Storrs, CT 06269-3060, USA. nicholas.leadbeater@uconn.edu

PMID: 17315069
DOI: 10.1039/b615597a

Abstract

Microwave-promoted esterification reactions have been monitored using in situ Raman spectroscopy. Having optimised a reaction on a 23 mmol scale, it was transferred to a larger reaction vessel and scaled up to 0.26 mol, again with Raman monitoring. With conditions in hand, an automated stop-flow apparatus was used to prepare 5.7 moles of product.