Reaktion #42531

ord-51725a07dc75426cb2d226d4e7ea7d78

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 2 h
  2. 2
    Einengenconcentrated under reduced pressure
  3. 3
    SonstigeThe resulting residue was partitioned between ethyl acetate and water
  4. 4
    WaschenThe organic layer was washed with saturated sodium chloride
  5. 5
    Trocknendried (sodium sulfate)
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated under reduced pressure

Vorschrift

A solution of 7-bromo-1-chloroisoquinoline (2.50 g, 10.3 mmol) and activated zinc (1.40 g, 21.65 mmol) in acetic acid (20 mL) was heated at reflux for 2 h. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. The resulting residue was partitioned between ethyl acetate and water. The organic layer was washed with saturated sodium chloride, dried (sodium sulfate), filtered, and concentrated under reduced pressure to provide 7-bromoisoquinoline (1.86 g): ESI MS m/z 208 [M+H]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727997B2uspto-grants-2010_06