Reaktion #364066

ord-05400052ced047f8a15bff83e575e081

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated under a reduced pressure
  2. 2
    workup.ADDITIONthe thus obtained residue was mixed with ethyl acetate and water
  3. 3
    ExtraktionThe reaction product was extracted with ethyl acetate
  4. 4
    Waschenwashed with saturated brine
  5. 5
    Trocknendried with anhydrous sodium sulfate
  6. 6
    SonstigeThen the compound obtained by the evaporation of the solvent under a reduced pressure
  7. 7
    Sonstigewas separated
  8. 8
    Sonstigepurified by a silica gel column chromatography

Vorschrift

2a-(4-Bromobutyl)-2a,3,4,5-tetrahydrobenz[cd]indole-2(1H)-one (220 mg, 0.72 mmol), 4-(2-methoxyphenyl)piperazine (150 mg, 0.79 mmol) and potassium carbonate (150 mg, 1.1 mmol) were stirred in anhydrous N,N-dimethylformamide (5 ml) at 50° C. for 4 hours. The solvent was evaporated under a reduced pressure, and the thus obtained residue was mixed with ethyl acetate and water. The reaction product was extracted with ethyl acetate, washed with saturated brine and dried with anhydrous sodium sulfate. Then the compound obtained by the evaporation of the solvent under a reduced pressure was separated and purified by a silica gel column chromatography to obtain 280 mg of the title compound (0.68 mmol, 94% in yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06355642B1uspto-grants-2002_03