反应详情

温度

10 °C

Bazedoxifene hydrochloride (20 g) and dimethylformamide (200 mL) are charged into a round bottomed flask and stirred for 10-15 minutes. To the reaction mixture, triethylamine (8 mL) and toluene (400 mL) are added and the mixture is stirred at room temperature for 10-20 minutes. Then two lots of water (40 mL and 860 mL) are sequentially added with intermittent stirring for 10-20 minutes and finally the reaction mixture is stirred for 5-6 hours at room temperature. The reaction mixture is then cooled to 7.5-12.5° C. and stirred at the same temperature for another 3-4 hours. The solid formed is collected by filtration, washed with water (40 mL), toluene (40 mL) and dried under vacuum below 50° C. to afford 16.2 g of crystalline bazedoxifene free base Form A of 99.79% HPLC purity.

1. stirringthe mixture is stirred at room temperature for 10-20 minutes
2. stirringwith intermittent stirring for 10-20 minutes
3. stirringfinally the reaction mixture is stirred for 5-6 hours at room temperature
4. stirringstirred at the same temperature for another 3-4 hours
5. customThe solid formed
6. filtrationis collected by filtration
7. washwashed with water (40 mL), toluene (40 mL)
8. customdried under vacuum below 50° C.