反応 #1687652

反応方程式

o-toluoyl chloride

1,4-dichlorobenzene

Aluminum chloride

→

white crystals

収率 36.0%

2,5-Dichloro-2'-methylbenzophenone

収率 36.0%

溶媒

Ether

反応条件

後処理

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
   その他The organic layer was separated
5. 5
   workup.DISTILLATIONdistilled under vacuum
6. 6
   その他after the removal of ether
7. 7
   workup.DISTILLATIONThe residue from distillation
8. 8
   その他was recrystallized twice from hexane

実験手順

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%).

出典