تفاعل #55955

ord-79b9351e6cbc4c129c78b56e06bd30c6

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
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
المردود 88.0%

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    درجة الحرارةThe temperature is maintained at 110° for 30 to 50 minutes
  3. 3
    أخرىwhen a solid is suddenly precipitated from the reaction mixture
  4. 4
    أخرىcompletion of the reaction
  5. 5
    درجة الحرارةto cool to room temperature
  6. 6
    أخرىthe product is collected
  7. 7
    غسيلwashed with ethanol
  8. 8
    أخرىto remove residual n-butyl acetate
  9. 9
    أخرىdried

الإجراء التجريبي

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.

المصدر

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