反応 #565293

ord-65cd0450302f40a4a7683d7e9e12f3f4

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度while heating
  2. 2
    温度under reflux for 41 hours
  3. 3
    workup.STIRRINGthe mixture stirred
  4. 4
    温度while heating
  5. 5
    温度under reflux for a further 19 hours
  6. 6
    その他the organic phase separated
  7. 7
    抽出The aqueous phase was extracted with toluene
  8. 8
    抽出the organic phases and toluene extract
  9. 9
    洗浄washed with water (2×100 parts)
  10. 10
    その他before evaporating

実験手順

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)].

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06641620B1uspto-grants-2003_11