Hydrogen Bromide → Nilotinib hydrobromide

Participants

Reaction Conditions

Reaction Steps

Nilotinib base (2.00 g, 3.77 mmol) was mixed with glacial acetic acid (8.00 mL, 4.0V). The mixture was heated to 40° C. with stirring which lead to a clear yellow solution. HBr 33% in acetic acid (0.8 mL, 4.53 mmol, 1.2 eq) was added in one portion to the stirred solution, leading to the formation of a yellow suspension. Stirring was continued at 40° C. over a period of 1 h. Due to the high viscosity of the mixture another 5 mL acetic acid (2.5V) was added. The mixture was then allowed to cool to room temperature by removal of the heat source, and the mixture was stirred at room temperature for an additional 4 h. The suspension was then filtered to give Nilotinib HBr form VI. The obtained product was dried in a vacuum oven (35 mmHg) at 40° C. for 3 days. The dried product was analyzed by PXRD and was found to be Nilotinib HBr form VI. The dried product was then subjected to additional drying at 60° C. in a vacuum oven for 15 hours, and then it was analyzed by PXRD and was found to be Nilotinib HBr form VI.

Provenance & Evidence