反应详情

To a mixture of 167 mg of 8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-3-carboxylic acid and 1.5 ml of dichloromethane was added 90 μl of 1-chloro-N,N,2-trimethylprop-1-en-1-amine under ice-cooling, followed by stirring at room temperature for 30 minutes. A solution of 93 mg of ethyl 2-amino-2-(pyrimidin-5-yl)propanoate in 1.5 ml of dichloromethane and 0.15 ml of triethylamine were added thereto under ice-cooling, followed by stirring at room temperature for 2 hours. To the reaction mixture was added water, followed by extraction with chloroform. 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 56 mg of ethyl 2-[({8-[(2,6-difluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridin-3-yl}carbonyl)amino]-2-(pyrimidin-5-yl)propanoate.

1. temperaturecooling
2. temperatureunder ice-cooling
3. stirringby stirring at room temperature for 2 hours
4. extractionfollowed by extraction with chloroform
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