HRID968792

反应详情

EQUATION

反应方程式

HRID 968792 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-amino-4-methyl-2-nitrobenzoic acid (16) (6.883 g, 35.10 mmol), 10% Pd/C [0.3 g, 10% dry Pd/C] and 75% aqueous formic acid (60 mL) is heated to reflux for about 15 hours. The reaction mixture is then cooled to ambient temperature and filtered through a pad of Celite, and the resulting filtrate concentrated in vacuo to a beige solid. The solids are triturated in hot methanol (50 mL), cooled slowly to ambient temperature, and filtered to give 7-Methyl-1H-benzimidazole-4-carboxylic Acid (22), as beige solid (5.26 g, 85% Yield).

WORKUP

后处理

  1. temperatureis heated
  2. temperatureto reflux for about 15 hours
  3. filtrationfiltered through a pad of Celite
  4. concentrationthe resulting filtrate concentrated in vacuo to a beige solid
  5. customThe solids are triturated in hot methanol (50 mL)
  6. temperaturecooled slowly to ambient temperature
  7. filtrationfiltered