Pieber Bartholomäus, Kappe C Oliver
Institute of Chemistry, University of Graz , NAWI Graz, Heinrichstrasse 28, A-8010 Graz, Austria.
Org Lett. 2016 Mar 4;18(5):1076-9. doi: 10.1021/acs.orglett.6b00194. Epub 2016 Feb 23.
A continuous process for the synthesis and inline separation of anhydrous trifluoromethyl diazomethane in a single continuous flow process is presented. The diazo building block is generated from the corresponding amine and NaNO2 under acidic, aqueous conditions and subsequently diffuses through a gas-permeable membrane into an organic stream. To avoid storage and transportation of the hazardous compound, a representative downstream process in a packed-bed reactor yielding highly functionalized building blocks was developed.
本文介绍了一种在单一连续流动过程中合成和在线分离无水三氟甲基重氮甲烷的连续方法。重氮结构单元在酸性水相条件下由相应的胺和亚硝酸钠生成,随后通过透气膜扩散到有机物流中。为避免危险化合物的储存和运输,开发了一种在填充床反应器中制备高官能化结构单元的典型下游工艺。