Reaktion #1114504

Reaktionsgleichung

1-(4-methylphenyl)pyrene

N-bromosuccinimide

dimethylformamide

→

1-bromo-6-(4-methylphenyl)pyrene

Ausbeute 22.4%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling the solution to room temperature
2. 2
   Extraktionfollowed by extraction with 500 ml of dichloromethane
3. 3
   WaschenThe organic layer was washed twice with 200 ml of water
4. 4
   Trocknendried over magnesium sulfate
5. 5
   Sonstigeevaporated
6. 6
   Filtrationfiltered
7. 7
   SonstigeThe filtrate was evaporated
8. 8
   Waschenthe residue was washed twice with 200 ml of ethyl acetate
9. 9
   FiltrationThe precipitated solid was collected by filtration
10. 10
    Sonstigevacuum-dried

Vorschrift

Next, a mixed solution of 40.0 g of 1-(4-methylphenyl)pyrene, 24.4 g of N-bromosuccinimide and 1.4 L of dimethylformamide was heated with stirring under a nitrogen gas flow at 40° C. for 7 hours. After cooling the solution to room temperature, 1.0 L of water was injected, followed by extraction with 500 ml of dichloromethane. The organic layer was washed twice with 200 ml of water, dried over magnesium sulfate, evaporated and then filtered using Celite. The filtrate was evaporated and the residue was washed twice with 200 ml of ethyl acetate. The precipitated solid was collected by filtration and then vacuum-dried to obtain 11.4 g of 1-bromo-6-(4-methylphenyl)pyrene.

Quelle