Reaktion #1757236
ord-d69012f647b04043bcfb39a3af3c3f44
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter the mixture was cooled to room temperature
- 2Extraktionthe mixture was extracted with 500 ml of dichloromethane
- 3WaschenThe organic layer was washed twice with 200 ml of water
- 4Trocknendried over magnesium sulfate
- 5Filtrationfiltered through celite
- 6SonstigeThe filtrate was evaporated
- 7Waschenthe resulting residue was washed twice with 200 ml of ethyl acetate
- 8SonstigeThe precipitated solid was separated by filtration
- 9Sonstigedried under vacuum
Vorschrift
A mixed solution of 40 g of 1-(4-methylphenyl)pyrene, 24.4 g of N-bromosuccinimide and 1.4 l of dimethylformamide was then heated and stirred at 40° C. for 7 hours under a nitrogen stream. After the mixture was cooled to room temperature, 1 l (liter) of water was added thereto, and the mixture was extracted with 500 ml of dichloromethane. The organic layer was washed twice with 200 ml of water, dried over magnesium sulfate, and then filtered through celite. The filtrate was evaporated, and the resulting residue was washed twice with 200 ml of ethyl acetate. The precipitated solid was separated by filtration and dried under vacuum to give 11.4 g of 1-bromo-6-(4-methylphenyl)pyrene.