تفاعل #565293

ord-65cd0450302f40a4a7683d7e9e12f3f4

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwhile heating
  2. 2
    درجة الحرارةunder reflux for 41 hours
  3. 3
    workup.STIRRINGthe mixture stirred
  4. 4
    درجة الحرارةwhile heating
  5. 5
    درجة الحرارةunder reflux for a further 19 hours
  6. 6
    أخرىthe organic phase separated
  7. 7
    استخلاصThe aqueous phase was extracted with toluene
  8. 8
    استخلاصthe organic phases and toluene extract
  9. 9
    غسيلwashed with water (2×100 parts)
  10. 10
    أخرىbefore evaporating

الإجراء التجريبي

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)].

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06641620B1uspto-grants-2003_11