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HRID918059

反应详情

EQUATION

反应方程式

HRID 918059 的结构方程式

REACTANTS

反应物

1
结构：C[C@]12CCC(=O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)COCCCCl)[C@@]3(C)CC(=O)[C@@H]12
HCID22791485

未命名化合物

PRODUCTS

生成物

1
结构：C[C@]12CC[C@@H](O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)COCCCCl)[C@@]3(C)CC(=O)[C@@H]12
HCID22791484

未命名化合物

收率 48.9%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：Cl.Cl.O.[Cl][Ir]([Cl])([Cl])[Cl]
催化剂HCID16211483

Tetrachloroiridium--hydrogen chloride--water (1/2/1)

H4Cl6IrO

PROCEDURE

实验过程

The less polar residue, crude 21-(3'-chloropropoxy)-5α-pregnane-3,11,20-trione (1.1 g.) was treated with `stock` chloroiridic acid solution. The mixture was then refluxed for 24 hours, cooled and partitioned between water and ether. The organic layer was washed with water, dried (Na2SO4) and evaporated. The residue was subjected to preparative t.l.c. EtOAc/petrol 1:1 to give title compound (0.54 g.) as a white foam, [α]D + 73° (c 1.3).

WORKUP

后处理

  1. temperatureThe mixture was then refluxed for 24 hours
  2. temperaturecooled
  3. custompartitioned between water and ether
  4. washThe organic layer was washed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated