Hydrochloric Acid → Nilotinib Hydrochloride Anhydrous

Participants

Reaction Conditions

Reaction Steps

To 1 Liter reactor was added Nilotinib-base form A (20 g, 0.04 mol), absolute ethanol (188 ml) and 13.77% HCl solution in ethanol abs. (10 g, 0.04 mol). The slurry was heated to reflux, mild dissolution occurred during the stirring, and the mixture was filtered under reduced pressure. During the filtration precipitation occurred. The precipitate was returned to the reactor. The mixture was heated to reflux until dissolution occurred at 65° C. and then cooled gradually to 55° C. During cooling, the solution precipitated at 60° C. The slurry was heated to reflux and cooled for 3 hours to 5° C. The slurry stirred at 5° C. over night, and ethanol abs. was added (100 ml) before filtration. The material filtered, washed with ethanol abs., and dried over night at 70° C. in vacuum oven to yield Nilotinib-HCl form T17 (19 g, 95% yield).

Provenance & Evidence