反应详情

温度

70 °C

Concentrated sulfuric acid (2.4 mL) was added to 2-amino-3,4-dihydropyrimidin-4-one (1 g, 9.0 mmol). The mixture was stirred and cooled in ice bath before dropwise addition of concentrated nitric acid (0.56 mL). The mixture was stirred at RT for 30 min before being heated at 70° C. for 2 hr. The mixture was allowed to cool to RT and was slowly added to water (10 mL), cooled in an ice bath. The resultant precipitate was collected by suction filtration, washed with diethyl ether (5 mL) and then thoroughly dried under high vacuum to give the title compound: 1H NMR (250 MHz, DMSO) δ 7.18 (1H, br. s.), 8.61 (1H, br. s.), 8.81 (1H, s); LC-MS: m/z=+156.9 (M+H)+.

1. temperaturecooled in ice bath
2. stirringThe mixture was stirred at RT for 30 min
3. temperatureto cool to RT
4. temperaturecooled in an ice bath
5. filtrationThe resultant precipitate was collected by suction filtration
6. washwashed with diethyl ether (5 mL)
7. customthoroughly dried under high vacuum