Реакция #55957

Уравнение реакции

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

Выход 83.5%

Растворители

n-butyl acetate

—

petroleum ether

Условия реакции

Обработка

1. 1
   Температураare heated
2. 2
   ТемператураThe temperature is maintained for 30 minutes
3. 3
   Другоеwhen reaction
4. 4
   ТемператураThe mixture is cooled to room temperature
5. 5
   ДругоеThe precipitate is collected
6. 6
   Промывкаwashed with petroleum ether (100 parts)
7. 7
   Другоеdried

Методика

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.

Источник