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

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

Nature protocols (2008-01-15)
Nicholas E Leadbeater, Jason R Schmink
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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
3-Acetylcoumarin, 96%
Sigma-Aldrich
Ethyl acetoacetate, Arxada quality, ≥99.0% (GC)
Sigma-Aldrich
Ethyl acetoacetate, natural, ≥97%, FG
Sigma-Aldrich
Ethyl acetoacetate, ≥99%, FCC, FG
Sigma-Aldrich
Ethyl acetoacetate, puriss. p.a., ≥99.0% (GC)
Sigma-Aldrich
Ethyl acetoacetate, ReagentPlus®, 99%