Reaktion #214929

Reaktionsgleichung

glyoxalic acid butyl ester

propionaldehyde

di-n-butylamine

→

3-formyl-crotonic acid butyl ester

Lösungsmittel

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONThe mixture is treated dropwise at 60° C. with 40.8 g
2. 2
   Sonstigerise higher than 105° C
3. 3
   Temperaturcooled
4. 4
   ExtraktionThe diethyl ether extract
5. 5
   Waschenis washed successively with 500 ml
6. 6
   Trocknenof water, dried over sodium sulphate
7. 7
   Sonstigeevaporated under reduced pressure
8. 8
   Sonstigeat 93°-105° C.

Vorschrift

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% of weight aqueous sodium bicarbonate solution and subsequently with 1000 ml. of water, dried over sodium sulphate and evaporated under reduced pressure. The remaining 3-formyl-crotonic acid butyl ester boils, after rectification, at 93°-105° C./14 mm. Hg.; nD25 =1.

Quelle