反应 #55956

ord-99c02245faa74ee4a81ad4cfc92bd3be

反应条件

温度
110°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heated
  2. 2
    温度The temperatures is maintained at 110° C. for 31/
  3. 3
    其他2 hours when reaction
  4. 4
    其他The solvent is removed at 80° C. under reduced pressure
  5. 5
    其他collected
  6. 6
    其他dried

实验过程

2-Bromo-4-nitro-4'-(N,N-diethylamino)azobenzene (1.9 parts), copper (I) iodide (0.95 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 temperatures is maintained at 110° C. for 31/2 hours when reaction is adjudged complete by thin layer chromatography. The solvent is removed at 80° C. under reduced pressure and the residue is slurried in water (250 parts), collected and dried. 2-Cyano-4-nitro-4'-(N,N-diethylamino)azobenzene is obtained in 75% yield and requires no purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04222935uspto-grants-1980_09