Reaktion #8089

ord-91f9a9d242cc4d829d962d9a6373321d

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto drop back to room temperature
  2. 2
    ExtraktionThe mixture was then extracted with ethyl acetate
  3. 3
    WaschenThe extract was washed with brine
  4. 4
    Trocknendried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    Sonstigethe residue was reacted

Vorschrift

To a solution of 4-methoxycarbonyl-6-[4-(methylthio)-phenyl]-2H-pyridazin-3-one (8.00 g, 29.0 mmol) in N,N-dimethylformamide (80 mL) were added potassium carbonate (8.02 g, 58.0 mmol) and isobutyl bromide (4.76 g, 34.8 mmol), and the mixture was stirred at 80° C. for 2 hours. The temperature of the reaction mixture was allowed to drop back to room temperature, and a saturated aqueous solution of sodium hydrogencarbonate was added. The mixture was then extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was distilled off. Following the procedure of Example 1 (7), the residue was reacted to yield the title compound as a yellow solid [yield: 65.1% (2 steps)].

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087606B2uspto-grants-2006_08