Reaktion #803778

ord-851d6f8eff904af0b96378e42a6ac6f6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was then evaporated
  2. 2
    Extraktionextracted with dichloromethane
  3. 3
    Trocknenthe organic layer was dried over magnesium sulfate
  4. 4
    Sonstigethe solvent was then evaporated
  5. 5
    SonstigeThe residue was then purified by column
  6. 6
    Sonstigev/v) as eluent and the product was further purified by recrystallization from toluene:ethanol (1:1
  7. 7
    Temperaturv/v), and after cooling
  8. 8
    Sonstige24.3 g (75%) of the product was collected as a white solid
  9. 9
    Filtrationafter filtration

Vorschrift

N-bromosuccinimide (17.8 g, 100 mmol) in DMF (50 mL) was added slowly to 9-(pyridin-2-yl)-9H-carbazole (24 g, 100 mmol) in THF (250 mL) at 0° C. over 30 min. The reaction was allowed to warm to room temperature and stir overnight. The reaction mixture was then evaporated and extracted with dichloromethane, and the organic layer was dried over magnesium sulfate and the solvent was then evaporated. The residue was then purified by column using toluene:hexane (1:1, v/v) as eluent and the product was further purified by recrystallization from toluene:ethanol (1:1, v/v), and after cooling, 24.3 g (75%) of the product was collected as a white solid after filtration.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09190623B2uspto-grants-2015_11