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HRID1973724

反应详情

EQUATION

反应方程式

HRID 1973724 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：O=C([O-])O.[K+]
HCID516893

Potassium bicarbonate

CHKO3

结构：CCOC(=CC=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@H](OC(C)=O)CC[C@]4(C)[C@H]3C(=O)C[C@]12C
HCID86734291

未命名化合物

PRODUCTS

生成物

1
结构：CCOC(=CC=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@H](O)CC[C@]4(C)[C@H]3C(=O)C[C@]12C
HCID86734290

未命名化合物

收率 34.1%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCO
溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

A solution of 3α-acetoxy-20-ethoxy-21-formyl-5α-pregn-20-en-11-one (500 mg) in ethyl alcohol (15 ml) was treated with potassium bicarbonate (450 mg) and the mixture was refluxed, under nitrogen, for 7 hours, then poured into water. The product was extracted with methylene chloride, and the extract washed with water, dried and evaporated. Purification of the residue (37 mg) by preparative t.l.c. and crystallisation from methyl acetate/petrol gave title compound (154 mg) m.p. 175°-178°, [α]D - 115.9°, λmax. 258 nm (ε 18,780).

WORKUP

后处理

  1. temperaturethe mixture was refluxed, under nitrogen, for 7 hours
  2. extractionThe product was extracted with methylene chloride
  3. washthe extract washed with water
  4. customdried
  5. customevaporated
  6. customPurification of the residue (37 mg) by preparative t.l.c
  7. customand crystallisation from methyl acetate/petrol