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HRID1973737

反应详情

EQUATION

反应方程式

HRID 1973737 的结构方程式

REACTANTS

反应物

3
结构：O
HCID962

Water

H2O

结构：O=C1NC(=O)c2ccccc21.[K]
HCID24194345

未命名化合物

结构：C[C@]12CC[C@@H](O)C[C@@H]1CC[C@H]1[C@@H]3CC[C@H](C(=O)CCCl)[C@@]3(C)CC(=O)[C@@H]12
HCID86734307

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)CCN4C(=O)c5ccccc5C4=O)[C@@]3(C)CC(=O)[C@@H]12
HCID22795163

未命名化合物

收率 63.3%

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-Chloromethyl-3α-hydroxy-5α-pregnane-11,20-dione (600 mg) in acetone was treated at reflux with potassium phthalimide (600 mg) for 10 hours, poured into water and the oily precipitate extracted into ether. The extracts were washed with water, dried over anhydrous sodium sulphate and evaporated to a white foam (700 mg). Purification by preparative t.l.c. in ethyl acetate/petrol (1:1) gave a foam which on trituration with ether gave title compound (490 mg) as a white solid m.p. 187°-189° [α]D + 58.8° (c = 0.97).

WORKUP

后处理

  1. extractionthe oily precipitate extracted into ether
  2. washThe extracts were washed with water
  3. dry with materialdried over anhydrous sodium sulphate
  4. customevaporated to a white foam (700 mg)
  5. customPurification by preparative t.l.c
  6. customin ethyl acetate/petrol (1:1) gave a foam which on trituration with ether