HRID1593032

反应详情

EQUATION

反应方程式

HRID 1593032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3[(3-bromophenyl)thio]propanoic acid (390 mg) and concentrated sulfuric acid (1.6 ml) was allowed to stand at 20° C. for 4 days. Water was added and the mixture was extracted with ethyl acetate. The organic solution was washed with sodium bicarbonate solution, brine, dried (MgSO4) and evaporated. The residue was purified by chromatography on a silica SPE cartridge (10 g) eluting with cyclohexane, dichloromethane-cyclohexane (1:2, 1:1) and dichloromethane to give the title compound (116 mg) 13C NMR δ (CDCl3) 193.5, 144.4, 131.0, 130.3, 130.0, 128.9, 128.8, 39.6, 27.1.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic solution was washed with sodium bicarbonate solution, brine
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customThe residue was purified by chromatography on a silica SPE cartridge (10 g)
  6. washeluting with cyclohexane, dichloromethane-cyclohexane (1:2, 1:1) and dichloromethane