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Flow Systems with a Packed-Bed Microreactor
A. R. Bogdan, B. P. Mason, K. T. Sylvester, D. T. McQuade*
Cornell University, Ithaca, USA
24 April 2007 (online)
Flow systems with packed-bed microreactors of resin-supported organocatalysts were developed. Flow systems consisted of fluoroelastomeric tubing (1.6 mm inner diameter) packed with functionalized Amberzyme oxirane (AO) resin, filter caps, and syringe pump. The Knoevenagel condensation of benzaldehyde with ethyl cyanoacetate was carried out in MeCN by using AO resin-supported 1,5,7-triazabicyclo-[4.4.0]undec-3-ene (AO-TBD) in packed-bed microreactor 1 to give ethyl trans-α-cyanocinnamate in 93% yield (0.2 g/h). The acylation of 1-phenylethanol was carried out in triethylamine (TEA) by using AO resin-supported DMAP (AO-DMAP) in packed-bed microreactor 2 to give the acylated product in 97% yield (1.6 g/h).