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HRID27679

反应详情

EQUATION

反应方程式

HRID 27679 的结构方程式

REACTANTS

反应物

4
结构：NC=O
HCID713

Formamide

CH3NO

结构：CCC(=O)OC(=O)CC
HCID31263

Propanoic anhydride

C6H10O3

结构：CCN(CC)c1ccc(N=Nc2c(Br)cc([N+](=O)[O-])cc2[N+](=O)[O-])c(NC(C)=O)c1
HCID104287

N-(2-((2-Bromo-4,6-dinitrophenyl)azo)-5-(diethylamino)phenyl)acetamide

C18H19BrN6O5

结构：CC(=O)[O-].[Na+]
HCID517045

Sodium Acetate

C2H3NaO2

PRODUCTS

生成物

1
结构：CCN(CC)c1ccc(N=Nc2c(C#N)cc([N+](=O)[O-])cc2[N+](=O)[O-])c(NC(C)=O)c1
HCID90383

N-(2-((2-Cyano-4,6-dinitrophenyl)azo)-5-(diethylamino)phenyl)acetamide

C19H19N7O5

收率 83.5%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Cu][I]
催化剂HCID24350

Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)

CuI

结构：CCCCOC(C)=O
溶剂HCID31272

Butyl acetate

C6H12O2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene (2.4 parts), copper (I) iodide (0.95 parts), anhydrous sodium acetate (1.2 parts), formamide (1.8 parts), propionic anhydride (2.6 parts) and n-butyl acetate (44 parts) are mixed together are heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained for 30 minutes when reaction is adjudged complete by thin layer chromatography. 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 83.5% yield.

WORKUP

后处理

  1. temperatureare heated
  2. temperatureThe temperature is maintained for 30 minutes
  3. customwhen reaction
  4. temperatureThe mixture is cooled to room temperature
  5. customThe precipitate is collected
  6. washwashed with petroleum ether (100 parts)
  7. customdried