Dimethyl Sulfoxide → HCID 86604014, compound

Participants

Reaction Steps

To 1.5 ml of a dimethylsulfoxide solution containing 174 mg (0.50 mmol) of 4-(2-aminopyridin-4-yl)-3-(4-fluorophenyl)-1-(1,6-dihydro-6-oxopyridazin-3-yl)-1H-pyrazole obtained by the same reaction as in Example 2-4) was added 0.3 ml of a dimethylsulfoxide solution containing 185 mg (1.05 mmol) of benzenesulfonic acid monohydrate at 45° C. over 15 minutes, and the mixture was stirred at the same temperature for 30 minutes. Then, 17 ml of ethyl acetate was added to the mixture over 10 minutes, and after gradually cooling the mixture to room temperature, the mixture was further stirred for 30 minutes. Formed crystals were collected by filtration, washed with 20 ml of ethyl acetate, and dried under reduced pressure to obtain 210 mg of the title compound as a white powder. (Yield: 83%)

Provenance & Evidence