Propanal → 3-Formyl-crotonic acid butyl ester

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.

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.

ORD record

ord-c1e89a141e0546a987eeead45c72ac2b

Source dataset

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04256878