Reaktion #1100935

ord-64bd13b296e841428a09b2c41c39ea98

Reaktionsbedingungen

Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to RT
  2. 2
    Sonstigequenched with saturated aqueous NaHCO3
  3. 3
    Sonstigeto precipitate a solid
  4. 4
    FiltrationThe solid was filtered
  5. 5
    Waschenwashed with water
  6. 6
    Sonstigedried

Vorschrift

A flask was charged with 4-(4-chlorophenyl)-N-(4-(6-methoxyquinolin-4-ylthio)phenyl)phthalazin-1-amine (0.325 g, 0.624 mmol), AcOH (5.71 ml, 99.8 mmol) and HBr (5.42 ml, 99.8 mmol). The mixture was stirred at 85° C. for 2 h, then cooled to RT and quenched with saturated aqueous NaHCO3 to precipitate a solid. The solid was filtered, washed with water and dried to give 4-(4-(4-(4-chlorophenyl)phthalazin-1-ylamino)phenylthio)quinolin-6-ol as a light yellow solid. MS: m/z=[M+H]+. 508.0 Calc'd for C29H19ClN4OS: 507.0.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07981891B2uspto-grants-2011_07