HRID247104

反应详情

EQUATION

反应方程式

HRID 247104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.4 g of N-acetyl-4-(2,3-dichlorophenyl)-3-trifluoromethylpyrrole, 15 ml of 25% aqueous ammonia solution and 60 ml of dioxane are stirred for 18 hours at 160° C. in an autoclave. The reaction mixture is cooled to room temperature and filtered, and the clear filtrate is concentrated by evaporation. The viscous residue is dissolved in ethyl acetate; the solution is washed firstly with water and then with a diluted sodium chloride solution; it is subsequently dried over sodium sulfate, filtered, and concentrated by evaporation. To the residue is added n-hexane, and the crystals which precipitate are filtered off and dried. The yield is 5.3 g of 4-(2,3-dichlorophenyl)-3-cyanopyrrole, m.p. 149°-150° C.

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationthe clear filtrate is concentrated by evaporation
  3. dissolutionThe viscous residue is dissolved in ethyl acetate
  4. washthe solution is washed firstly with water
  5. dry with materialit is subsequently dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated by evaporation
  8. additionTo the residue is added n-hexane
  9. filtrationthe crystals which precipitate are filtered off
  10. customdried