反应详情

Bazedoxifene hydrochloride (5 g), dichloromethane (75 mL), and water (50 mL) are mixed and triethylamine (4 mL) is slowly added to obtain a pH range of 9.5-10.5 of the aqueous phase. The layers are separated and the aqueous layer is extracted with dichloromethane (2×25 mL). The organic layers are combined followed by addition of water (50 mL), at which point pH of the aqueous phase is about 10.4. To this mixture, a solution of 5% acetic acid (75 mL) is slowly added until the pH is about 9, at which point a crystalline solid forms. The solid is collected by filtration, washed with dichloromethane (25 mL), and dried under vacuum at 50° C. to afford crystalline bazedoxifene free base in 73.27% yield (HPLC purity 99.67%).

1. customto obtain a pH range of 9.5-10.5 of the aqueous phase
2. customThe layers are separated
3. extractionthe aqueous layer is extracted with dichloromethane (2×25 mL)
4. additionThe organic layers are combined followed by addition of water (50 mL), at which point pH of the aqueous phase
5. additionTo this mixture, a solution of 5% acetic acid (75 mL) is slowly added until the pH is about 9, at which point a crystalline solid forms
6. filtrationThe solid is collected by filtration
7. washwashed with dichloromethane (25 mL)
8. customdried under vacuum at 50° C.