HRID1044183
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
A mixture of 2-chloro-1-(2,2-diethoxyethyl)-1H-benzimidazole (860 mg) and 3-(4-aminophenyl)-1-ethyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (636 mg) was heated at 150° C. for 50 min. The reaction mixture was partitioned between AcOEt/THF (1/1) and 1 M NaOH aqueous solution. The organic layer was separated, washed with brine, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography eluting with THF and recrystallized from THF to give 1-ethyl-3-[4-(1H-imidazo[1,2-a]benzimidazol-1-yl)phenyl]-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (311 mg).
WORKUP
后处理
- customThe reaction mixture was partitioned between AcOEt/THF (1/1) and 1 M NaOH aqueous solution
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure
- customThe residue was purified by basic silica gel column chromatography
- washeluting with THF
- customrecrystallized from THF