Reaktion #511590

ord-779e1f04f465485e9c3a84668290f801

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to ambient temperature
  2. 2
    Filtrationfiltered with suction
  3. 3
    Waschenrinsed with toluene
  4. 4
    SonstigeThe solid is recrystallized from N,N-dimethylformamide
  5. 5
    Waschenthe precipitate is washed with water
  6. 6
    Sonstigedried

Vorschrift

6.0 g (4-chloro-phthalazin-1-yl)-hydrazine (compound C1) are suspended in a mixture of 160 ml toluene and 18 ml triethylamine at 60° C. and treated with a solution of 6.0 g 4-methoxy-benzoyl chloride in 48 ml toluene. The mixture is stirred at 110° C. for 6 h, cooled to ambient temperature, filtered with suction and rinsed with toluene. The solid is recrystallized from N,N-dimethylformamide, the precipitate is washed with water and dried to yield 5.2 g of the title compound (m.p.: 192-193° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08106047B2uspto-grants-2012_01