Hydrogen Bromide → Nilotinib hydrobromide

Participants

Reaction Steps

Nilotinib base Form A (4.00 g, 7.55 mmol) was suspended in acetone (40 mL). The resulting mixture was stirred and heated to reflux for 0.5 h. HBr (48% aq., 0.88 mL, 7.78 mmol, 1.03 eq) was then added in one portion. The resulting mixture was refluxed for 10 min and then cooled to room temperature over 1 h. Then it was stirred at room temperature over 16 h and a solid precipitate formed. The solid was isolated by vacuum filtration and dried in a vacuum oven at 70° C. for 32 h to give Nilotinib HBr form XI as a yellow solid (4.42 g, 96%). Monohydrobromide salt was obtained according to assay determination.

Provenance & Evidence