反应详情

To a solution of 2-mercapto-5-methoxybenzimidazole (15.1 g, 0.14 mole) dissolved in 40 ml of 8.4% sodium hydroxide, was added 170 ml of methanol, followed by bromo(4-methoxy-3,5-dimethyl-2-pyridyl)acetonitrile (21.4 g, 0.11 mole) at room temperature. The mixture was heated to reflux for 1 h under a nitrogen atmosphere. The-resulting precipitate was removed by filtration and the methanol was evaporated. The residue obtained was extracted with chloroform, and the chloroform was washed 3 times with water and dried over magnesium sulfate. After evaporation of the solvent, the crude product was recrystallized from diethyl ether to give 22.6 g (90%) of the title compound as yellowish crystals: mp 193-197° C.; 1H NMR (CDCl3) δ 8.25 (s,1H), 7.65 (dd, 1H), 7.30 (m, 1H), 6.90 (m, 1H), 6.30 (br s, 2H), 3.95 (s, 3H), 3.75 (s, 3H), 2.50 (s, 3H), 2.20 (s, 3H) ppm.

1. temperatureThe mixture was heated
2. temperatureto reflux for 1 h under a nitrogen atmosphere
3. customThe-resulting precipitate
4. customwas removed by filtration
5. customthe methanol was evaporated
6. customThe residue obtained
7. extractionwas extracted with chloroform
8. washthe chloroform was washed 3 times with water
9. dry with materialdried over magnesium sulfate
10. customAfter evaporation of the solvent
11. customthe crude product was recrystallized from diethyl ether