Combined Raman and Microwave System: Monitoring a Multicomponent Reaction

The synthesis of new molecules is often sped up under high temperature and high pressure as provided by a microwave system. Raman spectroscopy is a helpful tool to monitor the progress and to determine the end-point of such chemical reactions in situ.

To demonstrate the potential of Anton Paar’s combined microwave and Raman setup, this report shows in situ monitoring of a Biginelli cyclocondensation building up a functionalized pyrimidine scaffold. During the reaction ethyl acetoacetate, an aryl aldehyde and urea are linked and yield a dihydropyrimidinone (DHPM). The Biginelli reaction is very tolerant regarding functionalization of all three starting materials and therefore allows access to a wide range of functionalized pyrimidines. As this building block occurs naturally in vitamins, nucleotides, pterins, and some natural antibiotics, access to an efficient synthesis route is highly desirable for the pharmaceutical and chemical industry.

This model system was chosen as an example for a typical multicomponent reaction as it is well understood and is widely used in industry. Combining a Cora 5001 Raman spectrometer with a Monowave 400 R gives the opportunity to monitor the reaction process and to determine the minimum reaction time.

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