Reaktion #514514

ord-29ff49fc865943db9649fa6387014393

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture heated
  2. 2
    Temperaturat reflux for 0.5 h
  3. 3
    Filtrationthe solid collected by filtration
  4. 4
    WaschenThe material was washed with ether
  5. 5
    Sonstigeazeotroped with ethanol
  6. 6
    Sonstigedried in vacuo
  7. 7
    Sonstigeto afford the title-compound

Vorschrift

1,4-Dichlorophthalazine (20.0 g, 0.100 mol) was added to a boiling solution of hydrazine monohydrate (37.3 ml, 0.765 mol) in ethanol (500 ml) and the mixture heated at reflux for 0.5 h. The mixture was cooled to room temperature and the solid collected by filtration. The material was washed with ether, azeotroped with ethanol and dried in vacuo to afford the title-compound. 1H NMR (250 MHz, d6-DMSO) δ 7.72-8.35 (4H, m, 4 of Ar—H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06313125B1uspto-grants-2001_11