Acetonitrile → HCID 54759637, compound

Participants

Reaction Conditions

Reaction Steps

N-(4-{4-amino-7-[1-(2-hydroxyethyl)-1H-pyrazol-4-yl]thieno[3,2-c]pyridin-3-yl}phenyl)-N′-(3-fluorophenyl)urea free base solid (26 mg) was suspended in dimethylformamide (125 μL) at 40° C. with magnetic stirring. Methanesulfonic acid (59 μL, 1 M) was slowly added to A-968660 free base suspension at 40° C. with magnetic stirring. Clear solution obtained after addition of methanesulfonic acid. Acetonitrile (150 μL) was then added to clear solution at 40° C. with magnetic stirring. Amorphous precipitation was observed shortly after the complete addition of the acid solution. The amorphous suspension was heated to 80° C. to obtain a clear solution, and then cooled spontaneously to ambient temperatures. Crystallization was observed upon cooling. Solid was collected by centrifuge filtration.

Provenance & Evidence