Dimethyl Sulfoxide → HCID 23633651, compound

Participants

Reaction Steps

To 1.5 ml of a dimethylsulfoxide solution containing 350 mg (1.00 mmol) of 4-(2-aminopyridin-4-yl)-3-(4-fluorophenyl)-1-(1,4,5,6-tetrahydro-6-oxopyridazin-3-yl)-1H-pyrazole obtained in Example 50 was added 130 μl (2.00 mmol) of methanesulfonic acid at 45° C. over 4 minutes, and the mixture was stirred at the same temperature for 30 minutes. Then, 4.5 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 30 ml of ethyl acetate to obtain 380 mg of the title compound as a white powder. (Yield: 85%)

Provenance & Evidence