Department of Chemistry, University of Connecticut, 55 North Eagleville Rd, Storrs, CT 06269-3060, USA.
Org Biomol Chem. 2011 Oct 7;9(19):6575-8. doi: 10.1039/c1ob05808h. Epub 2011 Aug 17.
A prototype tube-in-tube reactor in which it is possible to load gas and heat simultaneously has been used in a continuous-flow approach to alkoxycarbonylation reactions of aryl iodides. In the stainless steel coil, liquid flows on the outside of a gas-permeable membrane. The coil can be heated and the temperature can be measured accurately via a probe touching the outer steel surface. A range of aryl iodides can be transformed to the corresponding esters in excellent conversion by reaction at 120 °C using 0.5 mol% palladium acetate as the catalyst with no additional ligand required. Small-scale optimization and substrate screening runs were followed by scale-up.
一种原型管式反应器,可同时装入气体并加热,已用于连续流动的芳基碘烷氧基羰基化反应中。在不锈钢盘管中,液体在外层透气膜的外侧流动。盘管可以加热,通过探针接触外钢表面可以精确测量温度。一系列芳基碘化物在 120°C 下反应,以 0.5mol%醋酸钯作为催化剂,无需添加配体,即可转化为相应的酯,转化率非常高。在进行放大之前,先进行了小规模的优化和底物筛选实验。