反应详情

25 ml of methylamine solution (33% in ethanol) are diluted with 90 ml of dichloromethane. While cooling, 9.52 g (50 mmol) of 2,6-difluorophenylacetyl chloride dissolved in 10 ml of dichloromethane are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10°. The reaction mixture is stirred for a further hour at 10° and then extracted three times with water. The organic phase is dried over magnesium sulphate and concentrated. The crude product is recrystallised from dichloromethane/petroleum ether and yields 8.57 g (92.6% of the theoretical yield) of 2,6-difluorophenylacetic acid methylamide of m.p. 163°-164°.

1. temperatureWhile cooling
2. additionare added dropwise in such a manner that the temperature of the reaction mixture
3. customdoes not exceed 10°
4. extractionextracted three times with water
5. dry with materialThe organic phase is dried over magnesium sulphate
6. concentrationconcentrated
7. customThe crude product is recrystallised from dichloromethane/petroleum ether
8. customyields 8.57 g (92.6% of the