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HRID1077016

反应详情

EQUATION

反应方程式

HRID 1077016 的结构方程式

REACTANTS

反应物

4
结构：O
HCID962

Water

H2O

结构：[Na+].[OH-]
HCID14798

Sodium Hydroxide

HNaO

结构：S=c1cccc[nH]1
HCID2723698

2-Mercaptopyridine

C5H5NS

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

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)CSc4ccccn4)[C@@]3(C)CC(=O)[C@@H]12
HCID22790350

未命名化合物

收率 22.4%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：CCOCC
溶剂HCID3283

Diethyl Ether

C4H10O

结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

A solution of 21-bromo-3α-hydroxy-5α-pregnane-11,20-dione (1.0 g.) in tetrahydrofuran (10 ml) was added to a solution of pyrid-2-thione (0.5 g) in 2N-aqueous sodium hydroxide (10 ml). After allowing the mixture to stand at room temperature for 3 mins., water and ether were added. The organic layer was washed with water, dried (Na2SO4) and evaporated. The residue was subjected to preparative t.l.c. and recrystallisation from methyl acetate/petrol to give title compound (240 mg.) as white needles m.p. 184° [α]D + 130° (c 0.9).

WORKUP

后处理

  1. washThe organic layer was washed with water
  2. dry with materialdried (Na2SO4)
  3. customevaporated
  4. customand recrystallisation from methyl acetate/petrol