反应详情

61.1 g (0.314 mol) of 88% m-chloroperbenzoic acid are added to a suspension of 50.7 g (0.15 mol) of methyl 2-amino-6-[(p-toluenesulfonyl)oxy]-4-pyrimidinecarbamate in 1800 ml of methylene chloride and 300 ml of methanol. The solution, which becomes clear after 2 hours, is stirred at room temperature overnight and thereafter warmed to 40° for 8 hours. 1800 ml of hexane are added to this solution and the mixture is cooled to 0° overnight, whereby there forms a crystalline precipitate which is filtered off under suction and dried. The mother liquor is concentrated to approximately 400 ml under reduced pressure, there being obtained a further crystalline precipitate of methyl 2-amino-6-[(p-toluenesulfonyl)oxy]-4-pyrimidinecarbamate-3-oxide of melting point 144°-145°.

1. temperaturewarmed to 40° for 8 hours
2. temperaturethe mixture is cooled to 0° overnight
3. filtrationis filtered off under suction
4. customdried
5. concentrationThe mother liquor is concentrated to approximately 400 ml under reduced pressure, there