HRID428803

反应详情

EQUATION

反应方程式

HRID 428803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

26.5 g of 1-(4-chlorophenyl)-ethanol are added dropwise to 7.9 g of sodium hydride (55% in oil) in 250 ml of dimethylacetamide and the mixture is stirred at room temperature for 30 minutes. 25.7 g of 4-fluoropropiophenone are then added dropwise; the mixture is heated to 100° C. and stirred for 90 minutes. After cooling, the reaction mixture is concentrated in vacua; the residue is taken up in ethyl acetate, washed twice with water and once with saturated sodium chloride solution and dried over sodium sulfate. The solvent is evaporated off in vacuo and the residue is purified by recrystallisation from hexane to yield the title compound having a melting point 70-71° C.

WORKUP

后处理

  1. temperaturethe mixture is heated to 100° C.
  2. stirringstirred for 90 minutes
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture is concentrated in vacua
  5. washwashed twice with water and once with saturated sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. customThe solvent is evaporated off in vacuo
  8. customthe residue is purified by recrystallisation from hexane