反应详情

温度

140 °C

A mixture of 28.6 g (56 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-[6-chloro-4-(2-chloro-phenyl)-pyridin-3-yl]-N-methyl-isobutyramide, 50 ml dimethyl sulfoxide and 50 ml (830 mmol) ethanolamine was stirred at 140° C. for 24 h. The reaction mixture was cooled to room temperature, diluted with 200 ml ethyl acetate and washed with 200 ml 1 N sodium carbonate solution and 100 ml water. The aqueous layers were extracted with two 200-ml portions of ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated in vacuo. The residue was crystallized from a mixture of 150 ml diisopropyl ether and 150 ml heptane to give 29.1 g (93%) of the title compound as white crystals. M.p. 117-118° C.

1. temperatureThe reaction mixture was cooled to room temperature
2. washwashed with 200 ml 1 N sodium carbonate solution and 100 ml water
3. extractionThe aqueous layers were extracted with two 200-ml portions of ethyl acetate
4. dry with materialThe combined organic layers were dried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was crystallized from a mixture of 150 ml diisopropyl ether and 150 ml heptane