Reaktion #1787924

ord-5a6ab90d0f124cffb1b387207b238a05

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction solution was concentrated under reduced pressure
  2. 2
    Sonstigethe residue was recrystallized from ethanol-acetone

Vorschrift

To a mixture of 7-(2,5-dichlorothiophen-3-yl)-4-methyl-5,6,7,8-tetrahydrocinnolin-5-one (145 mg) and 1-amino-3-hydroxyguanidine hydrochloride (61 mg) were added ethanol (3 ml) and concentrated hydrochloric acid (0.05 ml), and the mixture was stirred at 90° C. for 1.5 hours. The reaction solution was concentrated under reduced pressure, and the residue was recrystallized from ethanol-acetone to give 7-(2,5-dichlorothiophen-3-yl)-5-(1-hydroxyguanidin-3-yl)imino-4-methyl-5,6,7,8-tetrahydrocinnoline hydrochloride (Compound 155) (80 mg) as whitish gray crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06350749B1uspto-grants-2002_02