Reaktion #1757236

ord-d69012f647b04043bcfb39a3af3c3f44

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter the mixture was cooled to room temperature
  2. 2
    Extraktionthe mixture was extracted 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
    Filtrationfiltered through celite
  6. 6
    SonstigeThe filtrate was evaporated
  7. 7
    Waschenthe resulting residue was washed twice with 200 ml of ethyl acetate
  8. 8
    SonstigeThe precipitated solid was separated by filtration
  9. 9
    Sonstigedried 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07989802B2uspto-grants-2011_08