HRID1973725

反应详情

EQUATION

反应方程式

HRID 1973725 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 21-ethoxycarbonyl-3α-hydroxy-5α-pregnane-11,20-dione 850 mg) in dry methyl alcohol (40 ml) was treated with potassium bicarbonate (1.02 g) and the mixture was refluxed, under nitrogen, for 1 hr., then poured into water. The product was extracted with ethyl acetate, and the extract washed with water, dried, and evaporated. The residue (506 mg) was purified by preparative t.l.c. and crystallisation from methyl acetate/petrol gave title compound (157 mg) m.p. 150°-152°, [α]D + 111.2°, λmax. 248.5 nm (ε 4,185).

WORKUP

后处理

  1. temperaturethe mixture was refluxed, under nitrogen, for 1 hr
  2. extractionThe product was extracted with ethyl acetate
  3. washthe extract washed with water
  4. customdried
  5. customevaporated
  6. customThe residue (506 mg) was purified by preparative t.l.c
  7. customand crystallisation from methyl acetate/petrol