HRID2235574
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
- 100 °C
PROCEDURE
实验过程
A mixture of 1.50 g (6.68 mmol) of methyl 2-chloro-1-methyl-1H-benzimidazole-7-carboxylate and 2.89 g (13.4 mmol) of 4-bromo-2-methoxy-6-methylphenylamine was heated at 100° C. for five days. The cooled reaction was dissolved in dichloromethane and washed with saturated aqueous sodium bicarbonate, water and brine. The organics were dried over sodium sulfate, filtered, and concentrated in vacuo. The thus obtained residue was purified via flash chromatography eluting with 100% dichloromethane to elute the residual 4-bromo-2-methoxy-6-methylphenylamine and 30% ethyl acetate/hexanes to give 356 mg (13%) of the title compound.
WORKUP
后处理
- customThe cooled reaction
- washwashed with saturated aqueous sodium bicarbonate, water and brine
- dry with materialThe organics were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe thus obtained residue was purified via flash chromatography
- washeluting with 100% dichloromethane
- washto elute the residual 4-bromo-2-methoxy-6-methylphenylamine and 30% ethyl acetate/hexanes