HRID1413749
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
A mixture of 8.96 g. of 3,4,5-tris(dimethylamino)-α-[(methylsulfonyl)methyl]benzyl alcohol, 2.56 g. of sodium methylate and 6.6 g. of β-anilinopropionitrile in 70 ml. of dimethylsulfoxide was stirred at room temperature under nitrogen for 50 minutes. The mixture was poured into 500 ml. of ice water, the separated oil extracted with ethyl acetate, the ethyl acetate solution dried over sodium sulfate and evaporated. By purification of the residue over aluminum oxide with benzene and recrystallization from ethanol, there was obtained α-(anilinomethylene)-3,4,5-tris(dimethylamino)hydrocinnamonitrile having a melting point of 179°-181° C.
WORKUP
后处理
- additionA mixture of 8.96 g
- additionThe mixture was poured into 500 ml
- extractionof ice water, the separated oil extracted with ethyl acetate
- dry with materialthe ethyl acetate solution dried over sodium sulfate
- customevaporated
- customBy purification of the residue over aluminum oxide
- customwith benzene and recrystallization from ethanol