반응 #55959

ord-a9221bcf0bbb4c9692966241d39232ec

반응 조건

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

후처리

  1. 1
    온도heated
  2. 2
    온도The temperature is maintained for 5 hours after which time the reaction
  3. 3
    온도The mixture is cooled to room temperature
  4. 4
    기타The precipitate is collected
  5. 5
    세척washed with petroleum-ether (100 parts)
  6. 6
    기타dried

실험 절차

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene (2.4 parts), copper (II) chloride (0.67 parts), anhydrous sodium acetate (1.2 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 for 5 hours after which time the reaction is complete. The mixture is cooled to room temperature and poured into petroleum-ether (boiling range 60-80°) (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 96% yield.

출처

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