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HRID1658419

反应详情

EQUATION

反应方程式

HRID 1658419 的结构方程式

REACTANTS

反应物

3
结构：CO
HCID887

Methanol

CH4O

结构：C[C@H](CCCC(C)(C)O)[C@H]1CC[C@H]2[C@@H]3CC[C@@]4(O)C[C@@H](O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID54528626

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@H](CCCC(C)(C)O)[C@H]1CC[C@H]2[C@@H]3CC[C@@]4(O)CC(=O)CC[C@]4(C)[C@H]3CC[C@]12C
HCID20739550

未命名化合物

收率 76.4%

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

A solution of 750 mg of the 3β ,5α -25-trihydroxy-cholestane (VI) in 300 ml of acetone was treated dropwise with 10cc of Jones reagent. The reaction mixture was treated with 10 ml of methanol, left for 15 minutes at room temperature and concentrated in vacuum. The residue was extracted with ether and washed with water. The ether extract was evaporated in vacuo and the residue was crystallized from benzene to give 570 mg of 3-keto-5α,25-dihydroxy-cholestane (VII) m.p. 215°-217°. Nmr δ 0.70 (s, 3H), 1.15 (s, 3H), 0.95 (d, J=5Hz, 1H), 1.22 (s, 3H) Anal. Calcd for C27H46O2 : C, 77.5; H, 11.1%. Found: C, 77.0; H, 10.5%.

WORKUP

后处理

  1. concentrationconcentrated in vacuum
  2. extractionThe residue was extracted with ether
  3. washwashed with water
  4. extractionThe ether extract
  5. customwas evaporated in vacuo
  6. customthe residue was crystallized from benzene