Reaktion #1527890

ord-2d123a315a074d19b7c5fe23cd715689

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONThe solution was poured onto ice water (600 ml)
  2. 2
    Sonstigethe precipitate was collected
  3. 3
    workup.DISSOLUTIONThe precipitate was dissolved in dichloromethane
  4. 4
    Waschenthe solution was washed with brine
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    Filtrationfiltered
  7. 7
    Sonstigethe filtrate was evaporated
  8. 8
    SonstigeThe residue was triturated with ethyl acetate
  9. 9
    Sonstigerecrystallized from chloroform-ether

Vorschrift

A solution of 2-chloro-5,6-dihydro-4H-imidazo[4,5,1-ij]quinoline (3.00 g), 4-(4-bromophenoxy)-3-phenylpiperidine (5.20 g), triethylamine (1.62 g) and dimethylformamide (50 ml) was stirred at 115° C., under nitrogen, overnight. The solution was poured onto ice water (600 ml) and the precipitate was collected. The precipitate was dissolved in dichloromethane and the solution was washed with brine, dried over anhydrous magnesium sulfate, filtered, and the filtrate was evaporated. The residue was triturated with ethyl acetate and then recrystallized from chloroform-ether to give 4.25 g (56%) of product, mp 188°-189° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05500423uspto-grants-1996_03