Reaktion #565293

ord-65cd0450302f40a4a7683d7e9e12f3f4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile heating
  2. 2
    Temperaturunder reflux for 41 hours
  3. 3
    workup.STIRRINGthe mixture stirred
  4. 4
    Temperaturwhile heating
  5. 5
    Temperaturunder reflux for a further 19 hours
  6. 6
    Sonstigethe organic phase separated
  7. 7
    ExtraktionThe aqueous phase was extracted with toluene
  8. 8
    Extraktionthe organic phases and toluene extract
  9. 9
    Waschenwashed with water (2×100 parts)
  10. 10
    Sonstigebefore evaporating

Vorschrift

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)].

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06641620B1uspto-grants-2003_11