Reaktion #55955

ord-79b9351e6cbc4c129c78b56e06bd30c6

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    TemperaturThe temperature is maintained at 110° for 30 to 50 minutes
  3. 3
    Sonstigewhen a solid is suddenly precipitated from the reaction mixture
  4. 4
    Sonstigecompletion of the reaction
  5. 5
    Temperaturto cool to room temperature
  6. 6
    Sonstigethe product is collected
  7. 7
    Waschenwashed with ethanol
  8. 8
    Sonstigeto remove residual n-butyl acetate
  9. 9
    Sonstigedried

Vorschrift

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino) azobenzene (479 parts), copper (I) iodide (19 parts), anhydrous sodium acetate (246 parts), formamide (180 parts), acetic anhydride (408 parts) and n-butyl acetate (2190 parts) are mixed together and heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained at 110° for 30 to 50 minutes, when a solid is suddenly precipitated from the reaction mixture, indicating completion of the reaction. The mixture is allowed to cool to room temperature and the product is collected, washed with ethanol to remove residual n-butyl acetate and dried. 2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene is obtained in 88% yield and requires no purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04222935uspto-grants-1980_09