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
CONDITIONS
反应条件
- 温度
- 113.5 °C
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
- additionThe mixture is treated dropwise at 60° C. with 40.8 g
- customrise higher than 105° C
- temperaturecooled
- extractionThe diethyl ether extract
- washis washed successively with 500 ml
- dry with materialof water, dried over sodium sulphate
- customevaporated under reduced pressure
- customat 93°-105° C.