反应 #1687652

ord-e2ef731d67a7486ab27da796c3a8819e

反应方程式

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
收率 36.0%
Cc1ccccc1C(=O)c1cc(Cl)ccc1Cl
2,5-Dichloro-2'-methylbenzophenone
收率 36.0%

溶剂

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05976437uspto-grants-1999_11