HRID1087186

反应详情

EQUATION

反应方程式

HRID 1087186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3'-chloro-4'-nitroacetophenone (2.7 g) in toluene (50 ml) was added to a stirred solution of lithium 2-(trifluoromethyl)thiophenoxide [4.4 g; Aust. J. Chem. 32 2313 (1979)]in ether (142 ml) at 0° C. The mixture was stirred at room temperature for 2 hours and refluxed for 20 minutes. The resulting mixtures were added ethyl acetate and water, and the organic layer was washed with water, dried and evaporated. The oily residue was purified by column chromatography on silica gel (70 g) eluting with toluene to give a yellow oil of 4'-nitro-3'-[2-(trifluoromethyl)phenylthio]acetophenone (1.3 g).

WORKUP

后处理

  1. customat 0° C
  2. temperaturerefluxed for 20 minutes
  3. washthe organic layer was washed with water
  4. customdried
  5. customevaporated
  6. customThe oily residue was purified by column chromatography on silica gel (70 g)
  7. washeluting with toluene