huagongshe.com
HRID1606345

反应详情

EQUATION

反应方程式

HRID 1606345 的结构方程式

REACTANTS

反应物

4
结构：[O-][Cl+3]([O-])([O-])O
HCID24247

Perchloric acid

HClO4

结构：O=P(O)(O)OP(=O)(O)OP(=O)(O)OP(=O)(O)O
HCID197147

Tetraphosphoric acid

H6O13P4

结构：N#C[S-].[K+]
HCID516872

Potassium thiocyanate

CKNS

结构：CC(=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@@H]5O[C@@H]5C[C@]4(C)[C@H]3C(=O)C[C@]12C
HCID86733130

未命名化合物

PRODUCTS

生成物

1
结构：CC(=O)[C@H]1CC[C@H]2[C@@H]3CC[C@H]4C[C@H](O)[C@@H](SC#N)C[C@]4(C)[C@H]3C(=O)C[C@]12C
HCID22789173

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：O
溶剂HCID962

Water

H2O

结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

2α,3α-Epoxy-5α-pregnane-11,20-dione (500 mg.) and potassium thiocyanate (2 g.) in dry tetrahydrofuran (40 ml.) were treated with tetraphosphoric acid (about 2 ml.), and the reaction was stirred at room temperature for 2 hours. Perchloric acid (60%, 0.1 ml.) was added, and after a further 30 minutes the solution was diluted with water and extracted with ether. The extract was washed with water, dried over sodium sulphate and evaporated to give a colourless oil which was purified by preparative tlc and recrystallisation from acetone/petrol to give the title compound, as white prisms m.p. 165°-170° [α]D + 78°.

WORKUP

后处理

  1. extractionextracted with ether
  2. washThe extract was washed with water
  3. dry with materialdried over sodium sulphate
  4. customevaporated
  5. customto give a colourless oil which
  6. customwas purified by preparative tlc and recrystallisation from acetone/petrol