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 absolute ethanol (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. Absolute ethanol was added (120 ml), and the precipitate was returned to the reactor. The mixture was heated to reflux until dissolution and stirred for 30 minutes, then cooled gradually to 5° C. over 3 h. While cooling, absolute ethanol was added (200 ml) and the slurry stirred at 5° C. for 30 minutes, filtered, washed with absolute ethanol, and dried over night at 70° C. in vacuum oven to yield Nilotinib-HCl form T17 (18.4 g, 83% yield).

Provenance & Evidence