反应详情

A solution of 4-chloro-1-difluoromethyl-1H-pyrazole-3-carboxylic acid (150 mg, 0.76 mmol) in dichloromethane (5 ml) was subsequently treated at 23° C. with N,O-dimethylhydroxylamine hydrochloride (78 mg, 0.80 mmol), N-methylmorpholine (0.09 ml, 0.8 mmol) and N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimide hydrochloride (154 mg, 0.8 mmol) and stirring was continued for 16 hours. The mixture was washed with 1 M aqueous hydrochloric acid and water, the organic layer was dried, evaporated and the residue purified by chromatography on silica gel using cyclohexane/ethyl acetate (2:1) as the eluent to give the title compound (164 mg) as a colorless oil. MS (ISP): m/z=240.1 [M]+.

1. washThe mixture was washed with 1 M aqueous hydrochloric acid and water
2. customthe organic layer was dried
3. customevaporated
4. customthe residue purified by chromatography on silica gel