HRID904452

反应详情

EQUATION

反应方程式

HRID 904452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

836 G. of the obtained glyoxalic acid butyl ester are introduced into 376 g. of propionaldehyde. The mixture is treated dropwise at 60° C. with 40.8 g. of di-n-butylamine. In so doing, the reaction temperature should not rise higher than 105° C. The reaction mixture is then stirred for 2 hours at 116°-111° C., cooled and taken up in ether. The diethyl ether extract is washed successively with 500 ml. of 1 N sulphuric acid, 700 ml. of water, 1000 ml. of 5% by weight aqueous sodium bicarbonate solution and subsequently with 1000 ml. of water, dried over sodium sulphate and evaporated under reduced pressure. The remaining 3-formylcrotonic acid butyl ester boils, after rectification, at 93°-105° C./14 mm. Hg.; nD25 =1.

WORKUP

后处理

  1. additionThe mixture is treated dropwise at 60° C. with 40.8 g
  2. customrise higher than 105° C
  3. temperaturecooled
  4. extractionThe diethyl ether extract
  5. washis washed successively with 500 ml
  6. dry with materialof water, dried over sodium sulphate
  7. customevaporated under reduced pressure
  8. customat 93°-105° C.