反应详情

温度

72.5 °C

Bazedoxifene acetate (2 g) and dimethylformamide (10 mL) are mixed and heated to 70-75° C. to produce a clear solution, followed by filtration. To the filtrate, toluene (400 mL), morpholine (1 mL), and water (100 mL) are added and the mixture is cooled to 0-10° C. and stirred overnight. The solid that forms is collected by filtration, washed with toluene (20 mL), and dried under vacuum below 80° C. for about 5 hours to afford crystalline bazedoxifene free base Form A (HPLC purity 99.2%, moisture content=0.32%).

1. customto produce a clear solution
2. filtrationfollowed by filtration
3. additionTo the filtrate, toluene (400 mL), morpholine (1 mL), and water (100 mL) are added
4. temperaturethe mixture is cooled to 0-10° C.
5. filtrationThe solid that forms is collected by filtration
6. washwashed with toluene (20 mL)
7. customdried under vacuum below 80° C. for about 5 hours