HRID1352884

反应详情

EQUATION

反应方程式

HRID 1352884 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2,4,6-trichloropyrimidine (5.00 g), 3,4-dichloroaniline (4.45 g, 1 equivalent) in 1,4-dioxane (20 mL) and N,N-diisopropylethylamine (10 mL) was heated at reflux with stirring for 3 hours. The solvent was removed and the crude material was purified by flash chromatography on silica gel. The column was eluted with a gradient of cyclohexane to ethyl acetate/cyclohexane (1:9). The eluent was removed, giving 4,6-dichloro-N-(3,4-dichlorophenyl)-2-pyrimidinamine (1.83 g, 58%, Rf=0.39 in ethyl acetate/cyclohexane, 2:3).

WORKUP

后处理

  1. temperatureat reflux
  2. customThe solvent was removed
  3. customthe crude material was purified by flash chromatography on silica gel
  4. washThe column was eluted with a gradient of cyclohexane to ethyl acetate/cyclohexane (1:9)
  5. customThe eluent was removed