Water → 1-tert-butyl-5-difluoromethoxy-3-trifluoromethyl-1H-pyrazole

To a solution of 10.4 g (50.0 mmol) of 1-tert-butyl-5-hydroxy-3-trifluoromethyl-1H-pyrazole in 50 ml of N,N-dimethylformamide was added 7.6 g (55.0 mmol) of anhydrous potassium carbonate at room temperature. While the reaction solution was stirred, an excess amount of chlorodifluoromethane was introduced into the reaction solution at 80° C. After the confirmation of disappearance of the starting material, the introduction of chlorodifluoromethane was stopped and the reaction solution was cooled to room temperature. Thereafter, the reaction solution was poured into water and extracted with diisopropyl ether. The resulting organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed by evaporation under reduced pressure and the residue was distilled under reduced pressure to obtain 10.8 g (yield: 83.7%) of 1-tert-butyl-5-difluoromethoxy-3-trifluoromethyl-1H-pyrazole as a yellow liquid.

1. extractionextracted with diisopropyl ether
2. washThe resulting organic layer was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent was removed by evaporation under reduced pressure
5. distillationthe residue was distilled under reduced pressure

ORD record

ord-ded08924ae8f4a799b02a2b4486c860d

Source dataset

uspto-grants-2007_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07256298B2