反应 #55957

反应方程式

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

收率 83.5%

溶剂

n-butyl acetate

—

petroleum ether

反应条件

后处理

1. 1
   温度are heated
2. 2
   温度The temperature is maintained for 30 minutes
3. 3
   其他when reaction
4. 4
   温度The mixture is cooled to room temperature
5. 5
   其他The precipitate is collected
6. 6
   洗涤washed with petroleum ether (100 parts)
7. 7
   其他dried

实验过程

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.

来源