Oxalic Acid → HCID 86688199, compound

Participants

Reaction Conditions

Reaction Steps

Nilotinib base Form A (4.00 g, 7.55 mmol) was suspended in EtOH abs. (40 mL, 10V) at room temperature. The suspension was heated to 80° C. and stirred at that temperature for 30 min. A solution of oxalic acid (1.38 g, 15.33 mmol, 2.03 mol eq) in EtOH abs. (10 mL 2.5V) was added in one portion and a suspension was obtained. Stirring of the suspension was continued for 1 h at 80° C. The reaction vessel was then allowed to cool to ambient temperature by removal of the reaction vessel from the heating source, and the mixture was stirred at ambient temperature for 6 h. Another 20 mL EtOH abs. was added during this time to improve the stirring. A yellow precipitate formed and was isolated by vacuum filtration and dried in a vacuum oven (35 mmHg) at 70° C. for 24 h to give Nilotinib oxalate form I (5.3 g) as a yellow solid. The sample was analyzed by PXRD (Bruker X-Ray powder diffractometer model D8 advance equipped with lynxEye). Di oxalate salt was obtained according to assay determination.

Provenance & Evidence