反应详情

温度

0 °C

A solution of 0.3 g (98 mmoles) of 8-phenyl-2-(4-pyridinyl)-6,7,8,9-tetrahydro-4H-pyrimido[1.2-a]pyrimidin-4-one in 8 ml of anhydrous dimethylformamide was treated with 51 mg (1.28 mmoles) of sodium hydride (60% in mineral oil). The resulting suspension was stirred at 0° C. for 30 mins and then treated with 0.255 g (1.28 mmoles) of 2-bromoacetophenone. After stirring for 18 h at room temperature, water was added and the reaction mixture was extracted with ethyl acetate. The organic phase was washed with a saturated solution of aqueous sodium chloride and was evaporated under reduced pressure to give crude product. Purification using silica gel chromatography eluting with a gradient comprising dichloromethane/methanol in the proportions 99/1 to 95/5 gave pure product which was dissolved in ethanol and treated with 1 equivalent of a solution of hydrochloric acid in isopropanol. The resulting salt was recrystallized from a mixture of isopropanol/diisopropylether to give 0.16 g (39%) of pure product. Mp: 134-137° C.

1. stirringAfter stirring for 18 h at room temperature
2. extractionthe reaction mixture was extracted with ethyl acetate
3. washThe organic phase was washed with a saturated solution of aqueous sodium chloride
4. customwas evaporated under reduced pressure
5. customto give crude product
6. customPurification
7. washeluting with a gradient comprising dichloromethane/methanol in the proportions 99/1 to 95/5
8. customgave pure product which
9. customThe resulting salt was recrystallized from a mixture of isopropanol/diisopropylether