HRID2379670

反应详情

EQUATION

反应方程式

HRID 2379670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

The damp N-acetyl-4-chloroanthranilic acid is suspended in 400 ml of concentrated hydrochloric acid (12M) and stirred and heated at 80° C. for 8 hours. The mixture is cooled to 10° C. and the resulting 4-chloroanthranilic acid hydrochloride is recovered by filtration. The solid is suspended in 300 ml water and sodium acetate is added, portionwise until the pH is 5. The resulting 4-chloroanthranilic acid is recovered by filtration and recrystallized from the minimum of hot ethanol. The final yield of off-white crystals was about 50 g, melting at about 239°-240° C.

WORKUP

后处理

  1. temperatureThe mixture is cooled to 10° C.
  2. filtrationthe resulting 4-chloroanthranilic acid hydrochloride is recovered by filtration
  3. additionsodium acetate is added, portionwise until the pH is 5
  4. filtrationThe resulting 4-chloroanthranilic acid is recovered by filtration
  5. customrecrystallized from the minimum of hot ethanol