HRID1668919

反应详情

EQUATION

反应方程式

HRID 1668919 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

3-Acetamido-4-methyl-2-nitrobenzoic acid (65 g, 273 mmol) was taken in dioxane (350 mL) and treated with 5 N aqueous HCl (150 mL). The reaction was stirred at 80° C. for 16 h. The dioxane was removed under reduced pressure and the residue poured onto crushed ice. The resulting precipitate was filtered off. The filtrate was extracted with ethyl acetate (2×). The organic layer and the solid were combined and concentrated under vacuum to give 3-amino-4-methyl-2-nitrobenzoic acid (45 g, 84% yield) as a yellow solid. MS (M+H)+ 197.

WORKUP

后处理

  1. customThe dioxane was removed under reduced pressure
  2. additionthe residue poured
  3. customonto crushed ice
  4. filtrationThe resulting precipitate was filtered off
  5. extractionThe filtrate was extracted with ethyl acetate (2×)
  6. concentrationconcentrated under vacuum