反应详情

After adding 63 g of 1,4-dioxa-8-azaspiro[4.5]decane and 13 ml of water to 17 g of 2α,3α-epoxy-16β-(1-pyrrolidinyl)-5α-androstane-17β-ol, the reaction mixture is maintained at 100° to 105° C. for 80 hours while introducing nitrogen. After completion of the reaction, the solution containing a precipitate is diluted with 200 ml of acetonitrile and after filtering, the precipitate is thoroughly washed with water and then with acetonitrile, dried and recrystallized from methanol to give the title product in a yield of 18.2 g (76.5%), m.p.: 184°-187° C.

1. temperaturethe reaction mixture is maintained at 100° to 105° C. for 80 hours
2. additionwhile introducing nitrogen
3. customAfter completion of the reaction
4. additionthe solution containing a precipitate
5. filtrationafter filtering
6. washthe precipitate is thoroughly washed with water
7. dry with materialwith acetonitrile, dried
8. customrecrystallized from methanol