HRID916079

反应详情

EQUATION

反应方程式

HRID 916079 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

Triethylamine (276 μl, 1.98 mmol) and 2-(bromoethyl)benzoic acid t-butyl ester (538 mg, 1.99 mmol) were added to 5,6-dimethylbenzimidazole-2-thiol (236 mg, 1.32 mmol) in 2 ml of dimethylformamide, which was then stirred at 80° C. for 3 hours. After the reaction was complete, water was added, followed by extraction with ethyl acetate. After drying the ethyl acetate phase with anhydrous sodium sulfate, it was concentrated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to obtain 2-((5,6-dimethylbenzimidazole-2-ylthio)methyl)benzoic acid t-butyl ester (288 mg, yield 59%).

WORKUP

后处理

  1. extractionfollowed by extraction with ethyl acetate
  2. dry with materialAfter drying the ethyl acetate phase with anhydrous sodium sulfate, it
  3. concentrationwas concentrated
  4. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)