反应详情

温度

40 °C

A solution containing 0.608 g (2.5 mmol) of 3-methyl-2-(pyrimidin-4-yl)-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one in anhydrous dimethylformamide was treated with 0.11 g (2.5 mmol) of sodium hydride (60% suspension in mineral oil) and the mixture warmed to 40° C. during 1 h. 0.497 g (2.5 mmol) of phenacyl bromide dissolved in 5 ml of dimethylformamide was added dropwise and the resulting solution stirred at room temperature for 3 h. The reaction mixture was treated with a saturated aqueous solution of sodium chloride and then extracted with ethyl acetate. The organic extracts were dried and evaporated to give a crude product, which was purified by chromatography on silica gel eluting with dichloromethane/methanol/ammonia in the proportions 100/0/0 to 98/2/0.2. A pure product was obtained which was triturated in diethylether to give 0.309 g (34%) of yellow solid. Mp.: 184-185° C.

1. additionwas added dropwise
2. extractionextracted with ethyl acetate
3. customThe organic extracts were dried
4. customevaporated
5. customto give a crude product, which
6. customwas purified by chromatography on silica gel eluting with dichloromethane/methanol/ammonia in the proportions 100/0/0 to 98/2/0.2
7. customA pure product was obtained which
8. customwas triturated in diethylether