反应详情

5,6-Diamino-1-cyclohexylmethyl-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one, (1.44 g, 5.67 mmol) together with triethyl orthoformate (15 mL) was heated at 146° C. for 2 h and 10 minutes. The mixture was allowed to cool to ambient temperature and then further cooled on an ice-bath, followed by addition of heptane (5 mL). After filtration of the suspension and washing with heptane (20 mL), the obtained solid was dried in vacuo. Suspending the solid (1.2 g) in a hot mixture of 2-propanol (125 mL), water (5 mL) and tert-butyl methyl ether (25 mL) gave, after cooling and filtration, a white precipitate which was washed with further tert-butyl methyl ether (5 mL). The solid was dried in vacuo to give the title compound (0.95 g, 63%).

1. temperaturefurther cooled on an ice-bath
2. filtrationAfter filtration of the suspension
3. washwashing with heptane (20 mL)
4. customthe obtained solid was dried in vacuo
5. additionin a hot mixture of 2-propanol (125 mL), water (5 mL) and tert-butyl methyl ether (25 mL)
6. customgave
7. temperatureafter cooling
8. filtrationfiltration
9. washa white precipitate which was washed with further tert-butyl methyl ether (5 mL)
10. customThe solid was dried in vacuo