反应详情

温度

22 °C

A solution of 1-difluoromethyl-1H-pyrazole-3-carboxylic acid (CAS925179-02-8) (500 mg, 3.1 mmole) in methanol (18 ml) was cooled to 0° C. and treated with sulphuric acid (98%, 0.2 ml, 3.1 mmol). The mixture was heated to reflux for 2 hours, cooled to 22° C. and concentrated at reduced pressure. The residue was partitioned between AcOEt and water, the organic layer was washed with water until the water phase showed a neutral pH, dried and evaporated to give the title compound (535 mg) as a colorless liquid which was used without further purification. MS: m/z=177.1 [M+H]+.

1. temperatureThe mixture was heated
2. temperatureto reflux for 2 hours
3. concentrationconcentrated at reduced pressure
4. customThe residue was partitioned between AcOEt and water
5. washthe organic layer was washed with water until the water phase
6. customdried
7. customevaporated