反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationfiltered
- concentrationthe clear filtrate is concentrated by evaporation
- dissolutionThe viscous residue is dissolved in ethyl acetate
- washthe solution is washed firstly with water
- dry with materialit is subsequently dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated by evaporation
- additionTo the residue is added n-hexane
- filtrationthe crystals which precipitate are filtered off
- customdried