Hydrogen Bromide → Nilotinib hydrobromide

Participants

Reaction Conditions

Reaction Steps

Nilotinib base Form A (3.50 g, 6.61 mmol) was suspended in EtOH (70 mL, 20V) and the resulting slurry was heated to 50° C. over 15 min with stirring. To the resulting pale yellow slurry was added HBr (48% aq., 1.23 g, 7.27 mmol, 1.1 eq) followed by another 2V of EtOH (7 mL). This addition led to a colour change to give a neon yellow suspension. The suspension was heated to reflux and another 18V EtOH (63 mL) was added portion-wise with stirring. After 1.5 h the suspension was removed from the heat source and stirred at room temperature overnight. After about 15 h the suspension was subjected to hot filtration (60° C.) under nitrogen. The mother liquors were separated from the solid and the collected solid was dried in a vacuum oven (35 mmHg) at 40° C. for 20 h to give Nilotinib HBr form IV (1.86 g) as a yellow solid.

Provenance & Evidence