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Use of Raman spectroscopy as a tool for in situ monitoring of microwave-promoted reactions

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Abstract

The progress of microwave-promoted reactions can be monitored by interfacing a Raman spectrometer with a scientific microwave unit. The apparatus is assembled from commercially available components. It is used in this protocol to follow the base-catalyzed reaction of salicylaldehyde with ethylacetoacetate to yield 3-acetylcoumarin. It is possible to watch the reaction spectroscopically in real time, determine when it reaches completion and thus use it as a tool for rapid reaction optimization.

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Figure 6: Screenshots of the real time Raman monitoring.
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Figure 9: Interfacing the Raman and microwave modules.
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Acknowledgements

We thank the University of Connecticut for research funding. We acknowledge technical support from CEM Corporation (in particular T. Michael Barnard) and Enwave Optronics (in particular Eric Wu and Kevin Pan).

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  1. Department of Chemistry, University of Connecticut, 55 North Eagleville Road, Storrs, 06269-3060, Connecticut, USA

    Nicholas E Leadbeater & Jason R Schmink

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  1. Nicholas E Leadbeater
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  2. Jason R Schmink
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Correspondence to Nicholas E Leadbeater.

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Leadbeater, N., Schmink, J. Use of Raman spectroscopy as a tool for in situ monitoring of microwave-promoted reactions. Nat Protoc 3, 1–7 (2008). https://doi.org/10.1038/nprot.2007.453

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