反应详情

Sodium (7.5 g) was added portionwise to a refluxing solution of 2β-ethoxy-17,17-ethylenedioxy-3α-hydroxy-5α-androstan-11-one 11-oxime (5.7 g) in propanol (400 ml) under nitrogen. Most of the solvent was evaporated in vacuo, water was added and the precipitated material was extracted into ethyl acetate. The washed extract was evaporated in vacuo and the residue was partitioned between ether and 2 N-hydrochloric acid. The aqueous layer was basified, extracted into ethyl acetate, washed, dried (Na2SO4) and evaporated to afford a froth which crystallized from ether to give the title compound m.p. 144°-148°, [α]D +61.5°.

1. customMost of the solvent was evaporated in vacuo, water
2. additionwas added
3. extractionthe precipitated material was extracted into ethyl acetate
4. extractionThe washed extract
5. customwas evaporated in vacuo
6. customthe residue was partitioned between ether and 2 N-hydrochloric acid
7. extractionextracted into ethyl acetate
8. washwashed
9. dry with materialdried (Na2SO4)
10. customevaporated
11. customto afford a froth which
12. customcrystallized from ether