Reaktion #8022

ord-0cf4acc0e65e454d8e4597bc7e4fb977

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted twice with chloroform (20 mL)
  2. 2
    WaschenThe extracts were washed with brine (20 mL)
  3. 3
    Trocknendried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONThe solvent was distilled off
  5. 5
    SonstigeThe residue was recrystallized from chloroform-hexane

Vorschrift

4-(4-tert-Butoxycarbonyl-1-piperazinyl)methyl-2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazine-3-one (220 mg, 0.47 mmol) was dissolved in ice-cold trifluoroacetic acid (2 mL), and at the same temperature, the mixture was stirred for 15 minutes. Water (10 mL) was added to the reaction mixture. The mixture was alkalinized with potassium carbonate and extracted twice with chloroform (20 mL). The extracts were washed with brine (20 mL) and dried over anhydrous sodium sulfate. The solvent was distilled off. The residue was recrystallized from chloroform-hexane to yield the title compound as pale yellow prisms (120 mg, 69.2%).

Quelle

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