HRID1413734

反应详情

EQUATION

反应方程式

HRID 1413734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9.76 g. of 3,5-bis(dimethylamino)-4-methoxy-α-[(methylsulfonyl)methyl]benzyl alcohol, 1.8 g. of sodium methylate and 4.8 g. of β-anilinopropionitrile in 20 ml. of dimethylsulfoxide was stirred with the exclusion of moisture for 5 hours at 50° C. The mixture was poured into 250 ml. of water, the precipitated oil extracted with ethyl acetate, the ethyl acetate solution dried over sodium sulfate and evaporated. By recrystallization of the residue from high-boiling petroleum ether, there was obtained α-(anilinomethylene)-3,5-bis(dimethylamino)-4-methoxyhydrocinnamonitrile, having a melting point of 103°-105° C.

WORKUP

后处理

  1. additionA mixture of 9.76 g
  2. additionThe mixture was poured into 250 ml
  3. extractionof water, the precipitated oil extracted with ethyl acetate
  4. dry with materialthe ethyl acetate solution dried over sodium sulfate
  5. customevaporated
  6. customBy recrystallization of the residue from high-boiling petroleum ether