反应详情

Phosphorus oxychloride (10 ml) was added to 1.5 g of 2-anilino-4-hydroxymethyl-6-methylpyrimidine and the mixture was heated under reflux for 15 minutes. After completion of the reaction, excessive phosphorus oxychloride was removed by distillation under reduced pressure. After dissolving the residue in dichloromethane, a 10% aqueous solution of sodium hydroxide was gradually added until the solution became alkaline under reflux of dichloromethane. After cooling to room temperature, the organic layer was washed with water, dried over magnesium sulfate and concentrated. The residual solid was recrystallized to obtain 1.2 g (yield: 73%) of 2-anilino-4-chloromethyl-6-methylpyrimidine having a melting point of 100°-101° C.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 15 minutes
3. customwas removed by distillation under reduced pressure
4. dissolutionAfter dissolving the residue in dichloromethane
5. additiona 10% aqueous solution of sodium hydroxide was gradually added until the solution
6. temperatureunder reflux of dichloromethane
7. washthe organic layer was washed with water
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated
10. customThe residual solid was recrystallized