반응 #3026

반응 방정식

Hydrogen chloride

m-toluoyl chloride

1,4-dichlorobenzene

Aluminum chloride

→

white crystals

수율 53.0%

2,5-Dichloro-3'-methylbenzophenone

수율 53.0%

용매

Ether

반응 조건

후처리

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

실험 절차

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%).

출처