Reaktion #7028

ord-cf6e582b3420469ba395e08f1c797454

Lösungsmittel

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeprepared in the Production Example 5
  2. 2
    TemperaturAfter the reaction solution was cooled to ambient temperature
  3. 3
    Waschenwas then washed with saturated aqueous sodium hydrogen carbonate solution
  4. 4
    TrocknenThe organic layer was dried over anhydrous magnesium sulfate
  5. 5
    SonstigeAfter the solvent was evaporated under reduced pressure
  6. 6
    Sonstigethe resulting solid was recrystallized from ethyl acetate

Vorschrift

In a sealed tube, N-(2-methoxyethyl)methylamine (3 ml) and water (3 ml) were added to 4-[3-bromo-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-4-yl]-2,1,3-benzooxadiazol (336 mg) prepared in the Production Example 5, and stirred at 160° C. for 6 hours. After the reaction solution was cooled to ambient temperature, chloroform was added to the solution, which was then washed with saturated aqueous sodium hydrogen carbonate solution. The organic layer was dried over anhydrous magnesium sulfate. After the solvent was evaporated under reduced pressure, the resulting solid was recrystallized from ethyl acetate, to afford the entitled compound as white crystal (66 mg, 19%). The physico-chemical values are as follows.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07084164B2uspto-grants-2006_08