HRID1606365

反应详情

EQUATION

反应方程式

HRID 1606365 的结构方程式

PROCEDURE

实验过程

2β-(2-Cyanoethoxy)-3α-hydroxy-5α-pregnane-11,20-dione (430 mg.) was dissolved in absolute ethanol (50 ml) and dry hydrogen chloride passed through the solution until saturation occurred. The mixture was left for one-fourth hour then poured into water (250 ml.). After one-half hour the precipitate formed was extracted into ether (2 × 100 ml), the ethereal solution washed with water and dried over anhydrous sodium sulphate. The dried solution was evaporated to a white form (320 mg) which was purified by preparative T.L.C. using ethyl acetate/petrol (4/1) run twice. The main band (Rf[0.4) gave title compound (140 mg) as an oil. [α]D + 61°(c, 0.5%).

WORKUP

后处理

  1. waitThe mixture was left for one-fourth hour
  2. customAfter one-half hour the precipitate formed
  3. extractionwas extracted into ether (2 × 100 ml)
  4. washthe ethereal solution washed with water
  5. dry with materialdried over anhydrous sodium sulphate
  6. customThe dried solution was evaporated to a white form (320 mg) which
  7. customwas purified by preparative T.L.C