反应详情

温度

78 °C

To a solution of 4-aminopyridin-2(1H)-one (Molbridge) (0.9 g, 8.17 mmol) in DMF (30 mL) was added NaH (60%, 490 mg, 12.3 mmol). The mixture was stirred at room temperature for 30 min before (2-bromoethoxy)(tert-butyl)dimethylsilane (2.15 g, 8.99 mmol) was added. The reaction mixture was heated at 78° C. for 15 h. The mixture was cooled and poured into H2O (100 mL) and extracted with ethyl acetate (3×50 mL). The organic layers were combined, washed with H2O (5×50 mL), brine (50 mL), dried over MgSO4 and concentrated. The residue was purified by flash chromatography (silica gel, 40+S, 0% to 10% MeOH in EtOAc) to give 4-amino-1-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-1H-pyridin-2-one as a white solid (0.9 g, 41%).

1. additionwas added
2. temperatureThe mixture was cooled
3. extractionextracted with ethyl acetate (3×50 mL)
4. washwashed with H2O (5×50 mL), brine (50 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated
7. customThe residue was purified by flash chromatography (silica gel, 40+S, 0% to 10% MeOH in EtOAc)