Reaktion #351770
ord-176befe930104a05a03f456cc17ed77b
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe mixture was heated to 170° C. in 30 min.
- 2TemperaturThe resulting brownish solution was cooled to about 80° C.
- 3workup.ADDITIONpoured onto ice
- 4SonstigeThe organic layer was separated
- 5workup.DISTILLATIONdistilled under vacuum
- 6Sonstigeafter the removal of ether
- 7workup.DISTILLATIONThe residue from distillation
- 8Sonstigewas recrystallized twice from hexane
Vorschrift
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%).