반응 #565293

ord-65cd0450302f40a4a7683d7e9e12f3f4

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while heating
  2. 2
    온도under reflux for 41 hours
  3. 3
    workup.STIRRINGthe mixture stirred
  4. 4
    온도while heating
  5. 5
    온도under reflux for a further 19 hours
  6. 6
    기타the organic phase separated
  7. 7
    추출The aqueous phase was extracted with toluene
  8. 8
    추출the organic phases and toluene extract
  9. 9
    세척washed with water (2×100 parts)
  10. 10
    기타before evaporating

실험 절차

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)].

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06641620B1uspto-grants-2003_11