反应详情

2-Methylthiobenzimidazole (0.50 g) was dissolved in dimethylformamide (10 ml), and sodium hydride (60% purity, oily) (0.13 g) was added thereto at room temperature. After stirring for 1 hour, 2-methylsulfonyl-4,6-dimethoxypyrimidine (0.67 g) was added at room temperature, followed by stirring for 8 hours. Ice water was added, followed by extraction with ethyl acetate, washing with a saturated sodium chloride aqueous solution and drying over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography to obtain 0.80 g of the desired product as a white powder (m.p. 135-137° C.)

1. customat room temperature
2. stirringby stirring for 8 hours
3. extractionfollowed by extraction with ethyl acetate
4. washwashing with a saturated sodium chloride aqueous solution
5. dry with materialdrying over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off
7. customthe residue was purified by silica gel column chromatography