Reaktion #582407

ord-4e651001aed24d878968717658c9e0e3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter heating to 90 C under nitrogen
  2. 2
    workup.ADDITIONwere added
  3. 3
    TemperaturThe reaction mixture was heated to 180 C for 4 hours
  4. 4
    Temperaturcooled to 130 C
  5. 5
    TemperaturAfter cooling to 5 C
  6. 6
    Filtrationthe product was filtered
  7. 7
    Waschenwashed with water
  8. 8
    SonstigeAfter drying

Vorschrift

To a flask were added 50 g polyphosphoric acid. After heating to 90 C under nitrogen, a mixture of 2.7 g 1,2-phenylenediamine and 2.1 g phthalic acid were added. The reaction mixture was heated to 180 C for 4 hours, then cooled to 130 C and poured into 150 ml water. The mixture was basified with aqueous ammonium hydroxide. After cooling to 5 C, the product was filtered and washed with water. After drying, 3.3 g of a gray solid remained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07538931B2uspto-grants-2009_05