Succinic Acid → Nilotinib succinate
反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:39])([F:38])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[C:40]([OH:47])(=[O:46])[CH2:41][CH2:42][C:43]([OH:45])=[O:44]>CN1C(=O)CCC1>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:21]([NH:23][C:24]2[CH:25]=[C:26]([C:36]([F:38])([F:39])[F:37])[CH:27]=[C:28]([N:30]3[CH:34]=[N:33][C:32]([CH3:35])=[CH:31]3)[CH:29]=2)=[O:22])=[CH:6][C:7]=1[NH:8][C:9]1[N:10]=[CH:11][CH:12]=[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[N:19][CH:20]=2)[N:14]=1.[C:40]([O-:47])(=[O:46])[CH2:41][CH2:42][C:43]([O-:45])=[O:44]参加物
4
反応条件
- 温度
- 80 °C
実験手順
Nilotinib base (0.5 g, 0.94 mmol) and succinic acid (0.144 g, 0.94 mmol) were mixed with NMP (1.5 mL, 3.0V). The mixture was stirred and heated to 80° C. to dissolution. The stirring was continued at the same temperature for 5 h, after which the mixture was allowed to cool to room temperature resulting in precipitation. The precipitate was separated by filtration to give Nilotinib succinate form III. The filter cake was then washed with EtOH (27 mL, 95%) and dried in a vacuum oven (30 mbar) at 40° C. for 16 h to give Nilotinib succinate form III (0.17 g) as an off-white solid.