HRID28669
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Thionyl chloride (10 mL, 0.137 mol) was added dropwise to a stirred suspension of the 1-bromophenyl-1H-benzimidazole-5-carboxylic acid (20 g, 0.063 mol) in MeOH (200 mL) at 0-5° C. The reaction was stirred at reflux for 18 h and then concentrated under reduced pressure. The solid residue was triturated with cold water, basified with aqueous ammonium hydroxide solution and extracted with DCM. The extract was washed with water, aqueous brine solution, dried over MgSO4 and concentrated in vacuo to give the corresponding 1-bromophenyl-1H-benzimidazole-5-carboxylic acid methyl ester: e.g. 1-(4-bromophenyl)-1H-benzimidazole carboxylic acid methyl ester.
WORKUP
后处理
- temperatureat reflux for 18 h
- concentrationconcentrated under reduced pressure
- customThe solid residue was triturated with cold water
- extractionextracted with DCM
- washThe extract was washed with water, aqueous brine solution
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo