Reaktion #1147767

ord-a80c100b29034a9caab5a688b6c27a70

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeobtained
  2. 2
    Temperaturunder reflux for 24 hours
  3. 3
    Temperaturcooled in ice
  4. 4
    Filtrationthe resultant precipitate was filtered
  5. 5
    Waschenwashed with ethanol and ethyl ether
  6. 6
    Sonstigedried under vacuum at 50° C.

Vorschrift

Hydrazine hydrate (0.81 ml, 0.84 g, 16.8 mmoles) was added to a solution under N2 of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (2 g, 5.6 mmoles), obtained as described in example 13, in ethanol (30 ml), and the mixture was kept under reflux for 24 hours, then cooled in ice and the resultant precipitate was filtered, washed with ethanol and ethyl ether and dried under vacuum at 50° C. to give 2.14 g of the title compound (stoichiometric yield). m.p.: 297-299° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06525055B1uspto-grants-2003_02