反应详情

5-Carbethoxy-2-mercapto-1H-benzimidazole (2.0 g, 9 mmol) and NaOH (0.36 g, 9 mmol) in H2O (1 ml) were dissolved in ethanol (30 ml). 3,4-dimethoxy-2-chloromethylpyridine hydrochloride (≈6.6 mmol) as a crude material were added and the mixture was heated to boiling. NaOH (0.26 g, 6.6 mmol) in H2O (1 ml) was added and the reflux was continued for 6 hours. The solvent was evaporated off and the residue was diluted with methylene chloride and water. The organic phase was dried over Na2SO4 and the solvent removed under reduced pressure. Crystallizing from CH3CN gave the desired product (1.75 g, 71%).

1. temperaturethe mixture was heated to boiling
2. customThe solvent was evaporated off
3. additionthe residue was diluted with methylene chloride and water
4. dry with materialThe organic phase was dried over Na2SO4
5. customthe solvent removed under reduced pressure
6. customCrystallizing from CH3CN