反应详情

3α,6α-Dihydroxy-5β-cholestan-24-one diacetate prepared in Example 2 was dissolved in a solution of potassium hydroxide (11 g) in methanol (200 ml), and the solution was stirred at room temperature for 3 hours. The reaction mixture was concentrated into about 50 ml in volume. Water was added to the concentrate and the separated oil was extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over magnesium sulfate and evaporated. The residue was chromatographed on silica gel to give 3 g of 3α,6α-dihydroxy-5β-cholestan-24-one having a melting point of 180°-181° C. after recrystallization from ethyl acetate.

1. concentrationThe reaction mixture was concentrated into about 50 ml in volume
2. additionWater was added to the
3. concentrationconcentrate
4. extractionthe separated oil was extracted with ethyl acetate
5. washThe ethyl acetate layer was washed with water
6. dry with materialdried over magnesium sulfate
7. customevaporated
8. customThe residue was chromatographed on silica gel