反应详情

To a solution of 0.450 g (1.10 mmol) of (+/−)-4-oxo-2-pyrimidin-4-yl-4,6,7,8,9,10-hexahydro-pyrimido[1,2-a]azepine-10-carboxylic acid 4-nitro-phenyl ester in 10 mL of dry acetonitrile in a sealed tube, were added 0.341 g (2.21 mmol) of 2,6-dimethoxy-pyridin-3-ylamine and 0.270 g (2.21 mmol) of dimethyl-pyridin-4-yl-amine. The resulting mixture was stirred under reflux for 16 hours. The mixture was dissolved in water and dichloromethane. The organic phases were washed with a saturated aqueous solution of sodium chloride, dried over sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography (dichloromethane/methanol/ammoniac in proportions of 100/0/0 to 98/2/02) to afford 0.121 g (26%) of a white solid.

1. temperatureunder reflux for 16 hours
2. washThe organic phases were washed with a saturated aqueous solution of sodium chloride
3. dry with materialdried over sodium sulfate
4. customevaporated to dryness
5. customThe residue was purified by flash chromatography (dichloromethane/methanol/ammoniac in proportions of 100/0/0 to 98/2/02)