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HRID1973717

反应详情

EQUATION

反应方程式

HRID 1973717 的结构方程式

REACTANTS

反应物

4
结构：CO
HCID887

Methanol

CH4O

结构：CCCC(=O)OCC
HCID7762

Ethyl butyrate

C6H12O2

结构：[H-].[Na+]
HCID24758

Sodium hydride

HNa

结构：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
HCID104845

Alphaxalone

C21H32O3

PRODUCTS

生成物

1
结构：CCCC(=O)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
HCID86734284

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CS(C)=O
溶剂HCID679

Dimethyl sulfoxide

C2H6OS

PROCEDURE

实验过程

Ethyl butyrate (0.84 ml) was added to a mixture of 3α-hydroxy-5α-pregnane-11,20-dione (665 mg) and sodium hydride (150 mg.) in dry dimethyl sulphoxide (10 ml.). The mixture was stirred, under N2, for 13/4 hrs. The reaction mixture was treated with methyl alcohol to destroy excess sodium hydride, then poured into 2N-hydrochloric acid. The product was extracted with ethyl acetate and the combined extracts were washed with water, dried and evaporated. Preparative t.l.c. of the residue (859 mg.) gave two fractions. The more polar fraction was title compound (244 mg.) [α]D + 74.0°, λmax. 278 nm (ε 12,980).

WORKUP

后处理

  1. customto destroy excess sodium hydride
  2. additionpoured into 2N-hydrochloric acid
  3. extractionThe product was extracted with ethyl acetate
  4. washthe combined extracts were washed with water
  5. customdried
  6. customevaporated
  7. customof the residue (859 mg.) gave two fractions