반응 #55957

반응 방정식

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

수율 83.5%

용매

n-butyl acetate

—

petroleum ether

반응 조건

후처리

1. 1
   온도are heated
2. 2
   온도The temperature is maintained for 30 minutes
3. 3
   기타when reaction
4. 4
   온도The mixture is cooled to room temperature
5. 5
   기타The precipitate is collected
6. 6
   세척washed with petroleum ether (100 parts)
7. 7
   기타dried

실험 절차

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.

출처