Reaktion #997024
ord-7b50f72126e84d199a01da325c719f37
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter heating to 90 C under nitrogen
- 2workup.ADDITIONwere added
- 3TemperaturThe reaction mixture was heated to 180 C for 4 hours
- 4Temperaturcooled to 130 C
- 5TemperaturAfter cooling to 5 C
- 6Filtrationthe product was filtered
- 7Waschenwashed with water
- 8SonstigeAfter 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.