Reaktion #1330068

ord-a74a646d666d435bb63d23877dcb60d4

Lösungsmittel

Reaktionsbedingungen

Temperatur
55°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    workup.STIRRINGwhich was stirred at room temperature for 72 hours
  3. 3
    Extraktionthe mixture alkaline, and extraction
  4. 4
    WaschenThe organic layer was washed with water and saturated aqueous sodium chloride solution
  5. 5
    Sonstigedried
  6. 6
    Einengenconcentrated
  7. 7
    SonstigeThe residue was recrystallized

Vorschrift

Anhydrous acetic acid (0.1 ml) was added to formic acid (1 ml), which was stirred at 55° C. for 2 hours. N-[3-[(N,N-dimethylamino)methyl]-1,2,3,4-tetrahydo-7-quinolinyl]-4-biphenylylcarboxamide (80 mg) was added to the reaction mixture under ice-cooling, which was stirred at room temperature for 72 hours. 10% aqueous potassium carbonate solution was added to the reaction mixture to make the mixture alkaline, and extraction was conducted using ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride solution, dried, and then concentrated. The residue was recrystallized using THF-IPE to give the titled compound (80 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07115750B1uspto-grants-2006_10