反应详情

温度

47.5 °C

Bazedoxifene free base (2 g) and acetone (20 mL) are mixed and heated to 45-50° C. to produce a clear solution, which is filtered. The filtrate is cooled to 25-35° C. and seed crystals (20 mg) are added, followed by drop-wise addition of acetic acid (0.26 g). n-Heptane (50 mL) is added drop-wise over 30 minutes. The formed solid is collected by filtration, sequentially washed with n-heptane (10 mL), and then suction dried for 5 minutes. The wet solid is dried under vacuum at 70° C. for about 4-5 hours to afford 1.5 g of crystalline bazedoxifene acetate Form D.

1. customto produce a clear solution, which
2. filtrationis filtered
3. temperatureThe filtrate is cooled to 25-35° C.
4. additionseed crystals (20 mg) are added
5. additionfollowed by drop-wise addition of acetic acid (0.26 g)
6. additionn-Heptane (50 mL) is added drop-wise over 30 minutes
7. filtrationThe formed solid is collected by filtration
8. washsequentially washed with n-heptane (10 mL)
9. customsuction dried for 5 minutes
10. customThe wet solid is dried under vacuum at 70° C. for about 4-5 hours