Реакция #55956

ord-99c02245faa74ee4a81ad4cfc92bd3be

Уравнение реакции

CCN(CC)c1ccc(N=Nc2ccc([N+](=O)[O-])cc2Br)cc1
2-Bromo-4-nitro-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=Nc2ccc([N+](=O)[O-])cc2C#N)cc1
2-Cyano-4-nitro-4'-(N,N-diethylamino)azobenzene
Выход 75.0%

Растворители

Условия реакции

Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated
  2. 2
    ТемператураThe temperatures is maintained at 110° C. for 31/
  3. 3
    Другое2 hours when reaction
  4. 4
    ДругоеThe solvent is removed at 80° C. under reduced pressure
  5. 5
    Другоеcollected
  6. 6
    Другоеdried

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04222935uspto-grants-1980_09