反应详情

温度

50 °C

2-Mercaptobenzimidazole (1.5 g) was dissolved in ethanol (20 ml) and thereto were added ethyl 2-dimethylamino-3-(2-chloromethyl-3-methyl-4-pyridylthio)propionate (3.16 g) and an aqueous solution (10 ml) of 1N sodium hydroxide. The mixture was stirred at 50° C. for 1 hour. The reaction mixture was concentrated under reduced pressure and water was added to the residue. The mixture was extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate and the solvent was distilled away under reduced pressure. The residue was subjected to column chromatography and eluted with chloroform-methanol to give 2-((3-methyl-4-(2-dimethylamino-2-ethoxycarbonylethylthio)-2-pyridyl)methylthio)-1H-benzimidazole as a pale yellow oil.

1. concentrationThe reaction mixture was concentrated under reduced pressure and water
2. additionwas added to the residue
3. extractionThe mixture was extracted with ethyl acetate
4. washThe extract was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled away under reduced pressure
7. washeluted with chloroform-methanol