反应详情

A solution of 17β, 19-dihydroxy-1α-methyl-4,6-androstadien-3-one diacetate in anhydrous tetrahydrofuran is slowly added to an ice cold ethereal solution of lithium dimethylcopper prepared as in the preceding Example. Stirring is continued for an additional 30 minutes and the mixture is poured onto a saturated aqueous ammonium chloride solution. Benzene is added and the mixture filtered through a bed of diatomaceous earth. The organic layer is separated, washed with aqueous ammonium chloride, washed with water, dried over magnesium sulfate and evaporated to dryness. The residue is chromatographed on a silica gel column and eluted with benzene. The eluant is evaporated and the residue recrystallized from a hexane solution to yield 17β,19-dihydroxy-1α,7α-dimethyl-5-androsten-3-one diacetate.

1. filtrationthe mixture filtered through a bed of diatomaceous earth
2. customThe organic layer is separated
3. washwashed with aqueous ammonium chloride
4. washwashed with water
5. dry with materialdried over magnesium sulfate
6. customevaporated to dryness
7. customThe residue is chromatographed on a silica gel column
8. washeluted with benzene
9. customThe eluant is evaporated
10. customthe residue recrystallized from a hexane solution