HRID2357713

反应详情

EQUATION

反应方程式

HRID 2357713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(4-chlorophenyl)pentane-1,4-dione (5.0 g., 0.024 mol, as obtained in Step-1) and 4-chloroaniline (3.33 g, 0.026 mol) in benzene (5.0 ml) was refluxed either over molecular sieves or using a Dean Stark apparatus. After three hours, benzene was removed under reduced pressure and the residue dissolved in ethyl acetate, washed with water (2×100 ml.) and brine (1×50 ml). The ethyl acetate layer was dried over anhydrous sodium sulfate, and the solvent evaporated off. The solid so obtained was washed with hexane to give 2.83 g (39.45%) of the title compound.

WORKUP

后处理

  1. temperaturewas refluxed either over molecular sieves
  2. custombenzene was removed under reduced pressure
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washwashed with water (2×100 ml.) and brine (1×50 ml)
  5. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  6. customthe solvent evaporated off
  7. customThe solid so obtained
  8. washwas washed with hexane