HRID906131

反应详情

EQUATION

反应方程式

HRID 906131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with water (10 mL)
  3. extractionThe aqueous mixture was extracted ethyl acetate (3×10 mL)
  4. extractionthe combined extract
  5. washwas washed with water (15 mL), brine (15 mL)
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated