تفاعل #1687652

ord-e2ef731d67a7486ab27da796c3a8819e

معادلة التفاعل

Cc1ccccc1C(=O)Cl
o-toluoyl chloride
Clc1ccc(Cl)cc1
1,4-dichlorobenzene
[Al+3].[Cl-].[Cl-].[Cl-]
Aluminum chloride
Cc1ccccc1C(=O)c1cc(Cl)ccc1Cl
white crystals
المردود 36.0%
Cc1ccccc1C(=O)c1cc(Cl)ccc1Cl
2,5-Dichloro-2'-methylbenzophenone
المردود 36.0%

الكواشف

لا شيء

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 o-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. 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 16 g of white crystals (36%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05976437uspto-grants-1999_11