反应详情

(2E)-3-(Dimethylamino)-1-pyrimidin-5-ylprop-2-en-1-one (1 g, 5.6 mmol) and N-(2-methyl-5-nitrophenyl)guanidine nitrate (1.44 g, 5.6 mmol) (Z. Szakacs et al., J. Med. Chem. 2005, 48, 249) were suspended in 20 mL of isopropanol. Sodium hydroxide (0.28 g, 7 mmol) was then added. The mixture solution was stirred overnight and cooled to room temperature. The solid was collected by filtration and rinsed with isopropanol and diethyl ether. The filtrate was concentrated under reduced pressure and the residue was dissolved in 15 mL of isopropanol. The solution obtained was refluxed overnight and cooled to room temperature. The solid was collected by filtration and rinsed with isopropanol and diethyl ether. The pooled solid was rinsed with water and diethyl ether, and dried in vacuum to obtain 1.2 g (70% yield) of the title compound. MS (M+1)=309.10.

1. filtrationThe solid was collected by filtration
2. washrinsed with isopropanol and diethyl ether
3. concentrationThe filtrate was concentrated under reduced pressure
4. dissolutionthe residue was dissolved in 15 mL of isopropanol
5. customThe solution obtained
6. temperaturewas refluxed overnight
7. temperaturecooled to room temperature
8. filtrationThe solid was collected by filtration
9. washrinsed with isopropanol and diethyl ether
10. washThe pooled solid was rinsed with water and diethyl ether
11. customdried in vacuum