反应详情

To a solution of 1.73 g of di-tert-butyl imidodicarbonate in DMF 16 ml was added 894 mg of potassium tert-butoxide under ice-cooling, followed by stirring at room temperature for 1 hour. To the reaction mixture was added a solution of 1.37 g of 3-bromo-4-(chloromethyl)pyridine in 3 ml of DMF under ice-cooling, followed by stirring at room temperature for 2 hours. To the reaction mixture was added water, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 2.32 g of di-tert-butyl [(3-bromopyridin-4-yl)methyl]imidodicarbonate.

1. temperaturecooling
2. temperaturecooling
3. stirringby stirring at room temperature for 2 hours
4. extractionfollowed by extraction with ethyl acetate
5. washThe organic layer was washed with water
6. dry with materiala saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
7. customthe solvent was then evaporated under reduced pressure
8. customThe obtained residue was purified by silica gel column chromatography