Reaktion #481594

ord-237bc96903554e8db12240565a2768d7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 1.5 hours
  2. 2
    TemperaturOn cooling
  3. 3
    Filtrationthe precipitate is collected by filtration
  4. 4
    Waschenwashed on the
  5. 5
    Filtrationfilter with ethanol, hot water and finally ethanol again
  6. 6
    SonstigeAfter drying
  7. 7
    Sonstigethis may be used without further purification (i.e. recrystallisation from benzene/methanol (1:1))

Vorschrift

A mixture of 2-ethylanthraquinone (25 Kg, 105.9 mol), NBS (19.1 Kg, 107.3 mol) and benzoyl peroxide (70%, 200 g, 0.58 mol) in CCl4 (˜150L) is stirred at reflux for 1.5 hours. On cooling, the precipitate is collected by filtration and washed on the filter with ethanol, hot water and finally ethanol again. After drying, this may be used without further purification (i.e. recrystallisation from benzene/methanol (1:1)).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06601732B1uspto-grants-2003_08