反应详情

A solution of 0.57 g (2.2 mmol) 1-(6-chloro-2-methyl-1H-indol-3-yl)-2,2,2-trifluoro-ethanone in 21.7 ml (86.8 mmol) aqueous 4 M sodium hydroxide solution was heated at reflux for 45 min. After cooling to room temperature the reaction mixture was diluted with water and extracted with tert-butyl methyl ether (2×50 ml). The aqueous layer was cooled to 0-5° C., acidified (pH 1-2) with concentrated aqueous hydrochloric acid solution and extracted with ethyl acetate (3×100 ml). The combined ethyl acetate layers were dried over sodium sulfate and concentrated in vacuo to give the title compound (0.14 g, 31%) as an off-white solid.

1. temperatureat reflux for 45 min
2. extractionextracted with tert-butyl methyl ether (2×50 ml)
3. temperatureThe aqueous layer was cooled to 0-5° C.
4. extractionextracted with ethyl acetate (3×100 ml)
5. dry with materialThe combined ethyl acetate layers were dried over sodium sulfate
6. concentrationconcentrated in vacuo