反应详情

0.26 ml of acetyl chloride is added to a mixture of 0.98 g of 1-(5-amino-2-pyridyl)-2-[2-(dimethylamino)benzylthio]imidazole, 1 ml of triethylamine and 30 ml of methylene chloride under ice-cooling. The mixture is stirred at the same temperature for 2 hours, washed with water and a saturated aqueous sodium bicarbonate solution, dried and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; chloroform:methanol=30:1), and crystallized with isopropyl ether. The crystals are collected by filtration, whereby 0.82 g of 1-(5-acetylamino-2-pyridyl)-2-[2-(dimethylamino)benzylthio]imidazole is obtained.

1. temperaturecooling
2. washwashed with water
3. dry with materiala saturated aqueous sodium bicarbonate solution, dried
4. customevaporated
5. customto remove the solvent
6. customThe residue is purified by silica gel column chromatography (solvent; chloroform:methanol=30:1)
7. customcrystallized with isopropyl ether
8. filtrationThe crystals are collected by filtration