HRID2404476
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of (3-bromophenyl)hydroxyacetic acid (809 mg) and 4,5-difluoro-ortho-phenylenediamine (500 mg) in 5N aqueous hydrochloric solution (2 mL) is heated under reflux for 15 h and cooled back to room temperature. The mixture is basified with concentrated sodium hydroxide and extracted with ethyl acetate. The organic phase is then dried over magnesium sulfate and concentrated under reduced pressure. The residue is purified by trituration in dichloromethane to afford the pure 3-bromophenyl(5,6-difluoro-1H-benzimidazol-2-yl)methanol.
WORKUP
后处理
- temperatureis heated
- temperatureunder reflux for 15 h
- extractionextracted with ethyl acetate
- dry with materialThe organic phase is then dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue is purified by trituration in dichloromethane