反应详情

To a solution of (6-chloro-indol-1-yl)-acetonitrile (0.446 g, 2.34 mmole) in acetonitrile (30 ml) was added dichloromethylene dimethylammonium chloride (phosgene imminium chloride) (0.418 g, 2.57 mmole). The reaction mixture was brought to reflux for 14 h and then poured into water (100 ml). The mixture was extracted into ethyl acetate and purified by column chromatography (silica gel, hexane:ethyl acetate 3:7) to afford the desired 6-chloro-1-cyanomethyl-1H-indole-3-carboxylic acid dimethylamide (0.286 g, 46% yield) in addition to recovered starting material (0.173 g). Step 3

1. temperatureto reflux for 14 h
2. extractionThe mixture was extracted into ethyl acetate
3. custompurified by column chromatography (silica gel, hexane:ethyl acetate 3:7)