Dimethyl Sulfoxide → HCID 69416617, compound

Participants

Reaction Steps

To 1.5 ml of a dimethylsulfoxide solution containing 430 mg (1.00 mmol) of 3-(4-fluorophenyl)-1-(1,6-dihydro-6-oxopyridazin-3-yl)-4-[2-(2,2,2-trifluoroethyl)aminopyridin-4-yl]-1H-pyrazole obtained in Example 28-2) was added 0.2 ml of 0.041M dil. sulfuric acid at 45° C. over 5 minutes, and the mixture was stirred at the same temperature for 1 hour. Then, 3.0 ml of ethyl acetate was added to the mixture over 30 minutes, and the resulting mixture was further stirred for 5 minutes. Formed crystals were collected by filtration, washed with 100 ml of ethyl acetate, and dried under reduced pressure to obtain 464 mg of the title compound as a white powder. (Yield: 88%)

Provenance & Evidence