HRID648889

反应详情

EQUATION

反应方程式

HRID 648889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 6.6 g (0.1 mol) of malononitrile in 100 ml of tetrahydrofuran was added 4.0 g (0.1 mol) of 60 wt% sodium hydride under ice-cooling. Seventeen grams (0.1 mol) of 6-chloro-1,3-dimethyluracil were added thereto, followed by stirring at room temperature for 5 hours. A hundred milliliters of water were added to the mixture, and the mixture was neutralized with concentrated hydrochloric acid, followed by extraction with 200 ml of ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was removed by distillation under reduced pressure, followed by filtration to obtain 12.9 g (63%) of 6-dicyanomethyl-1,3-dimethyluracil.

WORKUP

后处理

  1. temperaturecooling
  2. extractionfollowed by extraction with 200 ml of ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. customthe solvent was removed by distillation under reduced pressure
  5. filtrationfollowed by filtration