تفاعل #55957

ord-bd6608fb4bfe4cc9af4f818a4bca50c8

معادلة التفاعل

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
CCC(=O)OC(=O)CC
propionic 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
المردود 83.5%

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةare heated
  2. 2
    درجة الحرارةThe temperature is maintained for 30 minutes
  3. 3
    أخرىwhen reaction
  4. 4
    درجة الحرارةThe mixture is cooled to room temperature
  5. 5
    أخرىThe precipitate is collected
  6. 6
    غسيلwashed with petroleum ether (100 parts)
  7. 7
    أخرىdried

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04222935uspto-grants-1980_09