Reaktion #42540

ord-d676ac49f1b945c79fc6cf197f9470f2

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated under reduced pressure
  2. 2
    workup.ADDITIONThe residue was diluted with chloroform
  3. 3
    Waschenwashed with saturated sodium bicarbonate
  4. 4
    Trocknendried (sodium sulfate)
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated under reduced pressure
  7. 7
    Sonstigeto yield a brown oil
  8. 8
    SonstigePurification by flash column chromatography (silica, 3:1 hexanes/diethyl ether)

Vorschrift

A solution of 7-bromo-1-chloroisoquinoline (750 mg, 3.09 mmol) in N-methylbutylamine (7.0 mL) was heated at 65° C. in a sealed tube for 18 h. The reaction mixture was concentrated under reduced pressure. The residue was diluted with chloroform and washed with saturated sodium bicarbonate, dried (sodium sulfate), filtered, and concentrated under reduced pressure to yield a brown oil. Purification by flash column chromatography (silica, 3:1 hexanes/diethyl ether) provided 7-bromo-N-butyl-N-methylisoquinolin-1-amine (730 mg): ESI MS m/z 293 [M+H]+.

Quelle

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