反应详情

To a mixture of 3-[4-(6-methoxy-1-methyl-1H-benzimidazol-2-ylmethoxy)phenyl]-2-methylthiopropionic acid (1.1 g), tetrahydrofuran (15 ml) and dimethylformamide (15 ml) were added successively triethylamine (0.82 ml) and ethyl chloroformate (0.28 ml). The mixture was stirred at room temperature for 30 minutes. After addition of aqueous ammonia solution (5 ml, 28%) the mixture was stirred at room temperature for 15 minutes and allowed to stand overnight. The solvent of the reaction mixture was evaporated under reduced pressure. The residue was partitioned between ethyl acetate and water. The extract was washed with saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was washed with ethyl acetate and then recrystallized from a mixture of ethanol and ethyl acetate to afford the title compound (0.45 g, mp 204-206° C.).

1. stirringwas stirred at room temperature for 15 minutes
2. waitto stand overnight
3. customThe solvent of the reaction mixture was evaporated under reduced pressure
4. customThe residue was partitioned between ethyl acetate and water
5. washThe extract was washed with saturated aqueous sodium chloride solution
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. washThe residue was washed with ethyl acetate
9. customrecrystallized from a mixture of ethanol and ethyl acetate