HRID968792
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis heated
- temperatureto reflux for about 15 hours
- filtrationfiltered through a pad of Celite
- concentrationthe resulting filtrate concentrated in vacuo to a beige solid
- customThe solids are triturated in hot methanol (50 mL)
- temperaturecooled slowly to ambient temperature
- filtrationfiltered