HRID1973727

反应详情

EQUATION

反应方程式

HRID 1973727 的结构方程式

PROCEDURE

实验过程

3α-Hydroxy-21-methylene-5α-pregnane-11,20-dione (300 mg) was dissolved in thioacetic acid (2 ml) and left at room temperature for 3 hours. The mixture was poured into water and the precipitated oil extracted into ethyl acetate. The organic layer was washed with saturated sodium bicarbonate and water, dried over anhydrous sodium sulphate, evaporated to a pale yellow foam and purified by preparative t.l.c. in ethyl acetate/petrol (1:1). The main band gave title compound (150 mg) as an off-white foam. [α]D + 60.5° (c 0.98).

WORKUP

后处理

  1. extractionthe precipitated oil extracted into ethyl acetate
  2. washThe organic layer was washed with saturated sodium bicarbonate and water
  3. dry with materialdried over anhydrous sodium sulphate
  4. customevaporated to a pale yellow foam
  5. custompurified by preparative t.l.c