反应详情

10 Parts of 2-amino-4-(2,2-dichlorovinyl)-6-hydroxypyrimidine and 66 parts of phosphorus oxychloride were heated together under reflux for 1 hour with stirring. The solution was cooled and excess phosphorus oxychloride was removed in vacuo on a rotary evaporator. The residual viscous oil was poured onto ice, with stirring. Solid sodium bicarbonate was added portionwise until the solution had pH 7-8. The precipitated solid was filtered, washed with water and dried. Recrystallisation from aqueous methanol gave 2-amino-4-chloro-6-(2,2-dichlorovinyl)pyrimidine m.p. 119°-120° C.

1. temperatureunder reflux for 1 hour
2. temperatureThe solution was cooled
3. customexcess phosphorus oxychloride was removed in vacuo on a rotary evaporator
4. additionThe residual viscous oil was poured onto ice
5. stirringwith stirring
6. additionSolid sodium bicarbonate was added portionwise until the solution
7. filtrationThe precipitated solid was filtered
8. washwashed with water
9. customdried
10. customRecrystallisation from aqueous methanol