Hydrochloric Acid → Prasugrel Hydrochloride
反応式
[CH3:1][C:2]([O:4][C:5]1[S:9][C:8]2[CH2:10][CH2:11][N:12]([CH:14]([C:22]([CH:24]3[CH2:26][CH2:25]3)=[O:23])[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:20]=3[F:21])[CH2:13][C:7]=2[CH:6]=1)=[O:3].[ClH:27]>CC(C)=O>[CH3:1][C:2]([O:4][C:5]1[S:9][C:8]2[CH2:10][CH2:11][N:12]([CH:14]([C:22]([CH:24]3[CH2:26][CH2:25]3)=[O:23])[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:20]=3[F:21])[CH2:13][C:7]=2[CH:6]=1)=[O:3].[ClH:27]参加物
4
反応条件
- 温度
- 20 °C
実験手順
Prasugrel free base prepared by example 3 (2.0 g) disclosed herein was dissolved in acetone (25 ml) with stirring at 20° C. until complete dissolution and the mixture was further stirred for 10 minutes. A solution of hydrochloric acid in acetone (0.46 ml hydrochloric acid (37 wt. %) dissolved in 5 ml acetone) was added slowly to the reaction mixture over 1 hour at 20° C. After the addition, a seed crystal (0.05 g) (crystalline form B2 of prasugrel hydrochloride), the resulting mixture was stirred at 20° C. for 15 hours followed by filtration. The obtained crystal was washed with acetone and dried under vacuum at 50° C. for 24 hours. The resulting product was prasugrel hydrochloride crystalline Form B2 with the HPLC purity of 99.74%. The yield was 90%.