HRID620955

反应详情

EQUATION

反应方程式

HRID 620955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.0 g of 3-trifluoromethyl-4-(2,3-dichlorophenyl)pyrrole, 21 ml of 25% aqueous ammonia and 40 ml of dioxane are stirred for 26 hours at 180° C. in an autoclave. After cooling to room temperature, the reaction mixture is filtered, and the clear filtrate is concentrated by evaporation. The residue is taken up in ethyl acetate, washed with water and subsequently with diluted sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated by evaporation. The residue is caused to crystallise by the addition of hexane; it is then filtered off and dried to thus obtained 3.4 g (100% of theory) of 4-(2,3-dichlorophenyl)-3-cyanopyrrole having a melting point of 150° C.

WORKUP

后处理

  1. filtrationthe reaction mixture is filtered
  2. concentrationthe clear filtrate is concentrated by evaporation
  3. washwashed with water and subsequently with diluted sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation
  7. customto crystallise by the addition of hexane
  8. filtrationit is then filtered off
  9. dry with materialdried to thus obtained 3.4 g (100% of theory) of 4-(2,3-dichlorophenyl)-3-cyanopyrrole having a melting point of 150° C.