Dimethyl Sulfoxide → HCID 86604015, compound

Participants

Reaction Steps

To 50 ml of a dimethylsulfoxide solution containing 5.00 g (13.4 mmol) of 4-(2-aminopyridin-4-yl)-3-(4-fluorophenyl)-1-([1,2,4]triazolo[4,3-b]pyridazin-6-yl)-1H-pyrazole obtained by the same reaction as in Example 8-2) was added 2.35 ml (36.2 mmol) of methanesulfonic acid at 50° C. over 15 minutes, and the mixture was stirred at the same temperature for 1 hour. Then, 100 ml of ethyl acetate was added to the mixture over 10 minutes, and the resulting mixture was further stirred for 1 hour. Formed crystals were collected by filtration, washed with 150 ml of ethyl acetate, and dried under reduced pressure to obtain 5.80 g of the title compound as a beige powder. (Yield: 92%)

Provenance & Evidence