反应详情

A stirred mixture of 7-trifluoromethyl-5-(4-trifluoromethyl-phenyl)-pyrazolo[1,5-a]pyrimidine-3-carbonitrile [CAS-No. 851262-50-5] (2.0 g, 5.61 mmol), hydroxylamine hydrochloride (0.78 g, 11.2 mmol) and potassium carbonate (2.33 g, 16.8 mmol) in ethanol (100 ml) was heated under reflux conditions for 3 h. After the reaction mixture reached room temperature the precipitate was collected by filtration and washed with ethanol and ethyl acetate. The combined filtrates were evaporated and the crude product purified by flash chromatography on silica gel (ethyl acetate/heptane) to yield the title compound (1.51 g, 69%) as an orange solid. MS (ISP) 389.9 [(M+H)+]; mp 252° C.

1. temperaturewas heated under reflux conditions for 3 h
2. customreached room temperature
3. filtrationwas collected by filtration
4. washwashed with ethanol and ethyl acetate
5. customThe combined filtrates were evaporated
6. customthe crude product purified by flash chromatography on silica gel (ethyl acetate/heptane)