HRID1973725
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed, under nitrogen, for 1 hr
- extractionThe product was extracted with ethyl acetate
- washthe extract washed with water
- customdried
- customevaporated
- customThe residue (506 mg) was purified by preparative t.l.c
- customand crystallisation from methyl acetate/petrol