HRID968784

反应详情

EQUATION

反应方程式

HRID 968784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Phosphorus pentachloride (1.082 g) is added over about 30 minutes into a mixture of 4-methyl-3,5-dinitrobenzamide (6) (1.04 g) in acetonitrile (20 mL, 15 g). The mixture is then heated to about 60° C. for about 4 hours. The solution is then cooled to ambient temperature and is slowly added to an ice and water mixture (20 mL). The mixture is cooled to about 5° C., whereupon ammonium hydroxide is added until a pH of about 8 is attained. The product that precipitates is filtered, washed with water (10 mL), and dried to provide 4-methyl-3,5-dinitrobenzonitrile (4) (0.72 g, 75% Yield).

WORKUP

后处理

  1. temperatureThe solution is then cooled to ambient temperature
  2. additionis added until a pH of about 8
  3. customThe product that precipitates
  4. filtrationis filtered
  5. washwashed with water (10 mL)
  6. customdried