Reaktion #55958

ord-93bd652589b648a7801ab04648adafb1

Reaktionsgleichung

CCN(CC)c1ccc(N=Nc2c(Br)cc([N+](=O)[O-])cc2[N+](=O)[O-])c(NC(C)=O)c1
2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino) azobenzene
CC(=O)[O-].[K+]
potassium acetate
NC=O
formamide
CC(=O)OC(C)=O
acetic anhydride
CCN(CC)c1ccc(N=Nc2c(C#N)cc([N+](=O)[O-])cc2[N+](=O)[O-])c(NC(C)=O)c1
2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene
Ausbeute 95.0%

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    TemperaturThe temperature is maintained at 110° C. for 2 hours
  3. 3
    Sonstigewhen reaction
  4. 4
    TemperaturThe mixture is cooled to room temperature
  5. 5
    SonstigeThe precipitate is collected
  6. 6
    Waschenwashed with petroleum ether (100 parts)
  7. 7
    Sonstigedried

Vorschrift

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino) azobenzene (2.4 parts), copper (I) iodide (0.95 parts), anhydrous potassium acetate (1.5 parts), formamide (1.8 parts), acetic anhydride (2.0 parts) and n-butyl acetate (44 parts) are mixed together and heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained at 110° C. for 2 hours when reaction is complete. The mixture is cooled to room temperature and poured into petroleum ether (boiling range 60-80° C.) (400 parts). The precipitate is collected, washed with petroleum ether (100 parts) and dried. 2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene is obtained in 95% yield.

Quelle

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