反应详情

3α-Hydroxy-21-methylene-5α-pregnane-11,20-dione (500 mg) was dissolved in dioxan (40 ml) and dry hydrogen chloride passed through the solution for 1 hour. The mixture was left to stand for a further 2 hours, then poured into water and the sticky solid extracted into ether. The extracts were washed with saturated sodium bicarbonate, water and then dried over anhydrous sodium sulphate. After evaporation and trituration of the resulting foam with ether/petrol the title compound (375 mg) was obtained as a white solid. m.p. 110°-112° with gas evolution [α]D + 100° (c = 1.06).

1. waitThe mixture was left
2. extractionthe sticky solid extracted into ether
3. washThe extracts were washed with saturated sodium bicarbonate, water
4. dry with materialdried over anhydrous sodium sulphate
5. customAfter evaporation and trituration of the resulting foam with ether/petrol the title compound (375 mg)
6. customwas obtained as a white solid
7. custom100° (c = 1.06)