Reacción #214929

ord-c1e89a141e0546a987eeead45c72ac2b

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONThe mixture is treated dropwise at 60° C. with 40.8 g
  2. 2
    Otrorise higher than 105° C
  3. 3
    Temperaturacooled
  4. 4
    ExtracciónThe diethyl ether extract
  5. 5
    Lavadois washed successively with 500 ml
  6. 6
    Secadoof water, dried over sodium sulphate
  7. 7
    Otroevaporated under reduced pressure
  8. 8
    Otroat 93°-105° C.

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04256878uspto-grants-1981_03