Reaktion #155705

ord-c256786fceaf4707a367cfde7c1799e0

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder heat
  2. 2
    Temperaturunder heat
  3. 3
    TemperaturAfter having been cooled to room temperature
  4. 4
    WaschenThe resultant solid was sequentially washed with methanol, water, and methanol
  5. 5
    SonstigeAfter that, the solid was repeatedly recrystallized with toluene and hexane
  6. 6
    Waschenwashed

Vorschrift

First, 33.0 g of 2,6-diphenylanthracene were dissolved in 200 mL of N,N-dimethylformamide under heat, and then a solution of 18.0 g of N-bromosuccinimide in 20 mL of N,N-dimethylformamide was added to the solution. The mixture was stirred at 60° C. for 6 hours under heat. After having been cooled to room temperature, the reaction solution was poured into 1 L of water. The resultant solid was sequentially washed with methanol, water, and methanol. After that, the solid was repeatedly recrystallized with toluene and hexane and washed. Thus, 33.5 g of 9-bromo-2,6-diphenylanthracene were obtained (in 82% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822041B2uspto-grants-2014_09