反应详情

温度

-78 °C

To a solution tert-butyl 4-chloropyridin-2-ylcarbamate (2.29 g, 10 mmol), TMEDA (2.32 g, 20 mmol) in anhydrous THF (30 mL) was added n-BuLi (8 ml, 20 mmol). The resulting mixture was allowed to stir at −78° C. for 0.5 h which was added the solution of I2 (2.54 g, 10 mmol) in THF (8 mL) dropwise at −78° C. The reaction mixture was stirred for another 4 h. To the solution was added NH4Cl aq (5 mL), extracted with EtOAc (3×20 mL), dried over Na2SO4, filtered and concentrated. The crude residue was purified by column chromatography to afford the title compound as a yellow solid. LC/MS m/z=355.19 [M+H]+

1. stirringThe reaction mixture was stirred for another 4 h
2. extractionextracted with EtOAc (3×20 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe crude residue was purified by column chromatography