반응 #55955

ord-79b9351e6cbc4c129c78b56e06bd30c6

반응 조건

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

후처리

  1. 1
    온도heated
  2. 2
    온도The temperature is maintained at 110° for 30 to 50 minutes
  3. 3
    기타when a solid is suddenly precipitated from the reaction mixture
  4. 4
    기타completion of the reaction
  5. 5
    온도to cool to room temperature
  6. 6
    기타the product is collected
  7. 7
    세척washed with ethanol
  8. 8
    기타to remove residual n-butyl acetate
  9. 9
    기타dried

실험 절차

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.

출처

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