Reaktion #55957

Reaktionsgleichung

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene

sodium acetate

formamide

propionic anhydride

→

2-cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene

Ausbeute 83.5%

Lösungsmittel

n-butyl acetate

—

petroleum ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturare heated
2. 2
   TemperaturThe temperature is maintained for 30 minutes
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 sodium acetate (1.2 parts), formamide (1.8 parts), propionic anhydride (2.6 parts) and n-butyl acetate (44 parts) are mixed together are heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained for 30 minutes when reaction is adjudged complete by thin layer chromatography. 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 83.5% yield.

Quelle