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HRID1576793

反应详情

EQUATION

反应方程式

HRID 1576793 的结构方程式

REACTANTS

反应物

2
结构：C[C@]12CC[C@@H](O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)CBr)[C@@]3(C)CC(=O)[C@@H]12
HCID86733467

未命名化合物

结构：CC(C)=O.O=S(=O)(O)O.[O]=[Cr](=[O])=[O]
HCID131709961

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12CCC(=O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)CBr)[C@@]3(C)CC(=O)[C@@H]12
HCID86733474

未命名化合物

收率 85.4%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)=O
溶剂HCID180

Acetone

C3H6O

PROCEDURE

实验过程

21-Bromo-3α-hydroxy-5α-pregnane-11,20-dione (412 mg) in acetone (20 ml) was stirred during dropwise addition of Jones reagent (0.4 ml) at room temperature. After 10 minutes, the reaction mixture was poured onto water extracted with chloroform and the combined chloroform extract was washed with water dried (MgSO4) and evaporated. The residue was crystallised from ether/petrol to give title compound (350 mg) as white microcrystals mp 170° [αD ] + 132° (ε 1.1).

WORKUP

后处理

  1. additionthe reaction mixture was poured onto water
  2. extractionextracted with chloroform
  3. extractionthe combined chloroform extract
  4. washwas washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe residue was crystallised from ether/petrol