Whiffen Laboratory, University Chemical Laboratory, University of Cambridge, Lensfield Road, Cambridge, UK CB2 1EW.
Org Biomol Chem. 2011 Oct 21;9(20):6903-8. doi: 10.1039/c1ob06017a. Epub 2011 Aug 26.
We report on the development of a continuous flow process for the palladium catalysed methoxycarbonylation of aryl, heteroaromatic and vinyl iodides and an aryl bromide using a Teflon AF-2400 based Tube-in-Tube reactor to mediate the selective permeation of carbon monoxide into solution at elevated pressures. The low volume of pressurised gas within the reactor (5.6 mL) offers the potential for an enhanced safety profile compared to batch processes. We also present preliminary results for the use of in situ FTIR to measure solution concentrations of carbon monoxide and demonstrate the use of a second reactor to effect the removal of carbon monoxide from the flow stream.
我们报告了一种连续流动工艺的开发，该工艺使用 Teflon AF-2400 基 Tube-in-Tube 反应器作为媒介，在升高的压力下使一氧化碳选择性地渗透到溶液中，用于钯催化的芳基、杂芳基和乙烯基碘化物和芳基溴化物的甲氧羰基化。与分批工艺相比，反应器内加压气体的体积小（5.6 毫升），这为提高安全性提供了潜力。我们还介绍了使用原位 FTIR 测量一氧化碳溶液浓度的初步结果，并展示了使用第二个反应器从流中去除一氧化碳的效果。
