Reaktion #55956

Reaktionsgleichung

2-Bromo-4-nitro-4'-(N,N-diethylamino)azobenzene

sodium acetate

formamide

acetic anhydride

→

2-Cyano-4-nitro-4'-(N,N-diethylamino)azobenzene

Ausbeute 75.0%

Lösungsmittel

n-butyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   TemperaturThe temperatures is maintained at 110° C. for 31/
3. 3
   Sonstige2 hours when reaction
4. 4
   SonstigeThe solvent is removed at 80° C. under reduced pressure
5. 5
   Sonstigecollected
6. 6
   Sonstigedried

Vorschrift

2-Bromo-4-nitro-4'-(N,N-diethylamino)azobenzene (1.9 parts), copper (I) iodide (0.95 parts), anhydrous sodium acetate (1.2 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 temperatures is maintained at 110° C. for 31/2 hours when reaction is adjudged complete by thin layer chromatography. The solvent is removed at 80° C. under reduced pressure and the residue is slurried in water (250 parts), collected and dried. 2-Cyano-4-nitro-4'-(N,N-diethylamino)azobenzene is obtained in 75% yield and requires no purification.

Quelle