反应详情

To a solution of 4,6-diiodopyrimidin-5-amine (1.0 g) in tetrahydrofuran (10 mL) was added sodium hydride (60%, 138 mg) under ice-cooling. The mixture was stirred at room temperature for 30 min. To the reaction system was added dropwise a solution of methyl methanesulfonate (0.256 mL) in tetrahydrofuran (4.0 mL). The mixture was stirred at room temperature for 3 hrs and ethyl acetate was added. The mixture washed with water and saturated brine and dried over magnesium sulfate. After concentration under reduced pressure, the residue was separated and purified by silica gel column chromatography (hexane:ethyl acetate=9:1→3:1) to give the title compound (600 mg) as pale-yellow crystals.

1. temperaturecooling
2. stirringThe mixture was stirred at room temperature for 3 hrs
3. washThe mixture washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. concentrationAfter concentration under reduced pressure
6. customthe residue was separated
7. custompurified by silica gel column chromatography (hexane:ethyl acetate=9:1→3:1)