반응 #55958

ord-93bd652589b648a7801ab04648adafb1

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    온도The temperature is maintained at 110° C. for 2 hours
  3. 3
    기타when reaction
  4. 4
    온도The mixture is cooled to room temperature
  5. 5
    기타The precipitate is collected
  6. 6
    세척washed with petroleum ether (100 parts)
  7. 7
    기타dried

실험 절차

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino) azobenzene (2.4 parts), copper (I) iodide (0.95 parts), anhydrous potassium acetate (1.5 parts), formamide (1.8 parts), acetic anhydride (2.0 parts) and n-butyl acetate (44 parts) are mixed together and heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained at 110° C. for 2 hours when reaction is complete. 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 95% yield.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04222935uspto-grants-1980_09