Reaktion #366781

ord-71c6379b5a0e40a0ae01413bbc991edc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 2.5 hours
  3. 3
    Temperaturto cool
  4. 4
    Sonstigethe insoluble material removed by filtration
  5. 5
    SonstigeThe solvent was removed from the filtrate by evaporation
  6. 6
    Filtrationthe residue was purified by filtration through a silica pad
  7. 7
    Wascheneluting with ethyl acetate/hexane (10/1)

Vorschrift

A mixture of 2-bromo-4-methylpyridine (12.2 g), N-bromosuccinimide (30 g) and 2,2′-azobis(2-methylpropionitrile) (100 mg) in carbon tetrachloride (200 ml) was heated at reflux for 2.5 hours. The mixture was allowed to cool and the insoluble material removed by filtration. The solvent was removed from the filtrate by evaporation and the residue was purified by filtration through a silica pad eluting with ethyl acetate/hexane (10/1) to give 2-bromo-4-bromomethylpyridine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06362336B1uspto-grants-2002_03