Acetone → 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 hydrochloride salt

Participants

Reaction Steps

Acetone (451 uL) was added to the partially 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 (25.2 mg). Hydrochloric acid was added (1.1 equivalents; 1M in 1,4-dioxane), and the resulting mixture was temperature-cycled from 0-40° C. for a minimum of 48 hours. The product was filtered and dried in vacuo at room temperature. Yielded 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 HCl salt with a melting onset at 259° C. (determined by DSC).

Provenance & Evidence