تفاعل #3026

ord-4ed142657f3d431e82ca203fc86540a6

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated to 170° C. in 30 min.
  2. 2
    درجة الحرارةThe resulting brownish solution was cooled to about 80° C.
  3. 3
    workup.ADDITIONpoured onto ice
  4. 4
    أخرىThe organic layer was separated
  5. 5
    workup.DISTILLATIONdistilled under vacuum
  6. 6
    أخرىafter the removal of ether
  7. 7
    workup.DISTILLATIONThe residue from distillation
  8. 8
    أخرىwas recrystallized twice from hexane

الإجراء التجريبي

A mixture of m-toluoyl chloride (22 g, 0.17 mol) and 1,4-dichlorobenzene (120 g, 0.82 mol) was heated to 100° C. in a flask. Aluminum chloride (60 g, 0.45 mol) was added in one portion. Hydrogen chloride started to evolve from the solution. The mixture was heated to 170° C. in 30 min. and stirred at this temperature for 3 hours. The resulting brownish solution was cooled to about 80° C. and poured onto ice. Ether (50 ml) was added. The organic layer was separated and distilled under vacuum after the removal of ether. The residue from distillation was recrystallized twice from hexane to give 20 g of white crystals (53%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05731400uspto-grants-1998_03