反应详情

温度

27.5 °C

Bazedoxifene free base (2 g) and ethanol (4 mL) are mixed and stirred at 25-30° C. Acetic acid (2 mL) is added drop-wise and stirring is continued at the same temperature for 10 minutes. The mixture is cooled to 10-15° C., followed by drop-wise addition of diisopropyl ether (60 mL) and seed crystals (40 mg). The mixture is stirred at the same temperature for 10 minutes and the solid is collected by filtration, sequentially washed with diisopropyl ether (20 mL) and water (5 mL), and suction dried for 5 minutes. The obtained wet solid is dried under vacuum at 70° C. for about 4-5 hours to afford 1.7 g of crystalline bazedoxifene acetate Form D. HPLC purity=99.46%, moisture content=0.61%.

1. stirringstirring
2. temperatureThe mixture is cooled to 10-15° C.
3. stirringThe mixture is stirred at the same temperature for 10 minutes
4. filtrationthe solid is collected by filtration
5. washsequentially washed with diisopropyl ether (20 mL) and water (5 mL), and suction
6. customdried for 5 minutes
7. customThe obtained wet solid is dried under vacuum at 70° C. for about 4-5 hours