HRID906131
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
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
A mixture of the methyl 1,4-dimethyl-1H-benzimidazole-5-carboxylate (78 mg, 0.38 mmol) in methanol (2 mL) and 5% aqueous sodium hydroxide solution (2 mL) was stirred at 60° C. for one hour. The reaction mixture was concentrated, diluted with water (10 mL) and the pH adjusted to 4 then saturated with solid sodium chloride. The aqueous mixture was extracted ethyl acetate (3×10 mL) and the combined extract was washed with water (15 mL), brine (15 mL), dried over sodium sulfate, filtered and concentrated to give 1,4-dimethyl-1H-benzimidazole-5-carboxylic acid (46 mg, 63% yield), MS (EI) for C10H10N2O2: 191 (MH+).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- additiondiluted with water (10 mL)
- extractionThe aqueous mixture was extracted ethyl acetate (3×10 mL)
- extractionthe combined extract
- washwas washed with water (15 mL), brine (15 mL)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated