Reacción #524792

ord-054609431cda4882a1a5d0fc4bcd9d80

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe mixture was heated
  2. 2
    Temperaturaunder reflux for 12 hours
  3. 3
    Extracciónextracted several times with a 10% sodium hydroxide solution
  4. 4
    LavadoThe organic layer was washed with water
  5. 5
    Secadodried (Na2SO4)
  6. 6
    Otrothe solvent removed under reduced pressure
  7. 7
    Otroto give a pale brown oil which
  8. 8
    Otrocrystallised

Procedimiento

Crotonyl chloride (7 ml) was added to a solution of 2,4-dichloro-6-nitrophenol (10.3 g) in methylene chloride (20 ml) and the mixture was heated under reflux for 12 hours. The solution was diluted with further methylene chloride (200 ml) and extracted several times with a 10% sodium hydroxide solution. The organic layer was washed with water dried (Na2SO4) and the solvent removed under reduced pressure to give a pale brown oil which crystallised on standing for 24 hours 2,4-dichloro-6-nitrophenyl crotonate melted at <60°.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04031249uspto-grants-1977_06