Acetonitrile → 3-[2-{[3-(Diethylamino)-propyl]amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-n-propylbenzamide ethanedisulfonate salt hydrate

Participants

Reaction Conditions

Reaction Steps

Acetonitrile (450 uL) was added to the crystalline 3-[2-{[3-(diethylamino)propyl]-amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide-free-base (25.0 mg), and the resulting mixture was heated to 50° C. Ethanedisulfonic acid was added (1.1 equivalents; 1M in methanol). The mixture was cooled to room temperature and stirred several hours. The product was filtered and dried for at least one hour in a vacuum oven at 50° C. with a slow nitrogen bleed. The yield was 62.0% (20.7 mg) of 3-[2-{[3-(diethylamino)-propyl]amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide ethanedisulfonate salt hydrate with a melting onset at <100° C. (determined by DSC).

Provenance & Evidence