HRID648889
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
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
- temperaturecooling
- extractionfollowed by extraction with 200 ml of ethyl acetate
- dry with materialThe extract was dried over anhydrous sodium sulfate
- customthe solvent was removed by distillation under reduced pressure
- filtrationfollowed by filtration