Reacción #565293

ord-65cd0450302f40a4a7683d7e9e12f3f4

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawhile heating
  2. 2
    Temperaturaunder reflux for 41 hours
  3. 3
    workup.STIRRINGthe mixture stirred
  4. 4
    Temperaturawhile heating
  5. 5
    Temperaturaunder reflux for a further 19 hours
  6. 6
    Otrothe organic phase separated
  7. 7
    ExtracciónThe aqueous phase was extracted with toluene
  8. 8
    Extracciónthe organic phases and toluene extract
  9. 9
    Lavadowashed with water (2×100 parts)
  10. 10
    Otrobefore evaporating

Procedimiento

A mixture of N-(1-methylhexyl)aniline (76 parts), 1-bromobutane (66 parts), anhydrous potassium carbonate (65 parts) and DMF (150 parts) was stirred while heating under reflux for 41 hours. An additional quantity of 1-bromo butane (44 parts) was added and the mixture stirred while heating under reflux for a further 19 hours. The cooled mixture was poured into water (400 parts) and the organic phase separated. The aqueous phase was extracted with toluene, the organic phases and toluene extract were combined and washed with water (2×100 parts) before evaporating to leave N-butyl-N-(1-methylhexyl)aniline (72.8 parts, 44%) which was purified by vacuum distillation to give N-butyl-N-(1-methylhexyl)aniline b.pt 73-80° C., 2.6 mm Hg. [Dye (1)].

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06641620B1uspto-grants-2003_11