Реакция #55955

ord-79b9351e6cbc4c129c78b56e06bd30c6

Уравнение реакции

CCN(CC)c1ccc(N=Nc2c(Br)cc([N+](=O)[O-])cc2[N+](=O)[O-])c(NC(C)=O)c1
2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino) azobenzene
CC(=O)[O-].[Na+]
sodium acetate
NC=O
formamide
CC(=O)OC(C)=O
acetic anhydride
CCN(CC)c1ccc(N=Nc2c(C#N)cc([N+](=O)[O-])cc2[N+](=O)[O-])c(NC(C)=O)c1
2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene
Выход 88.0%

Растворители

Условия реакции

Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated
  2. 2
    ТемператураThe temperature is maintained at 110° for 30 to 50 minutes
  3. 3
    Другоеwhen a solid is suddenly precipitated from the reaction mixture
  4. 4
    Другоеcompletion of the reaction
  5. 5
    Температураto cool to room temperature
  6. 6
    Другоеthe product is collected
  7. 7
    Промывкаwashed with ethanol
  8. 8
    Другоеto remove residual n-butyl acetate
  9. 9
    Другоеdried

Методика

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino) azobenzene (479 parts), copper (I) iodide (19 parts), anhydrous sodium acetate (246 parts), formamide (180 parts), acetic anhydride (408 parts) and n-butyl acetate (2190 parts) are mixed together and heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained at 110° for 30 to 50 minutes, when a solid is suddenly precipitated from the reaction mixture, indicating completion of the reaction. The mixture is allowed to cool to room temperature and the product is collected, washed with ethanol to remove residual n-butyl acetate and dried. 2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene is obtained in 88% yield and requires no purification.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04222935uspto-grants-1980_09