反应详情

温度

0 °C

5α-Pregnane 3,20-dione (10 g) is reacted with a reagent obtained by reacting FeCl3 (5.2 g) and MeMgCl (4 equiv, based on FeCl3) in anhydrous tetrahydrofuran (200 mL) at −25° C. for 3 h. The reaction is quenched with acetic acid (32 ml). The reaction mixture is concentrated in vacuo and the residue is stirred with 3N HCl for 6 h. The solid is collected by filtration, washed with water and dried at 50° C. under vacuum to obtain crude ganaxolone. The crude product is dissolved in THF (33 mL) at reflux and filtered hot. The filtrate is added with water (45 mL) to obtain a suspension, which is collected by filtration, washed with water and dried. The dried product is further slurried in ethyl acetate (50 mL) at 70° C. for 19 h. The suspension is cooled to 0° C. and filtered, washed with cold ethyl acetate and dried to obtain ganaxolone.

1. customobtained
2. customat −25° C.
3. customfor 3 h
4. customThe reaction is quenched with acetic acid (32 ml)
5. concentrationThe reaction mixture is concentrated in vacuo
6. filtrationThe solid is collected by filtration
7. washwashed with water
8. customdried at 50° C. under vacuum
9. customto obtain crude ganaxolone
10. temperatureat reflux
11. filtrationfiltered hot
12. additionThe filtrate is added with water (45 mL)
13. customto obtain a suspension, which
14. filtrationis collected by filtration
15. washwashed with water
16. customdried
17. waitThe dried product is further slurried in ethyl acetate (50 mL) at 70° C. for 19 h
18. filtrationfiltered
19. washwashed with cold ethyl acetate
20. customdried