反应详情

温度

150 °C

A solution of 7.6 g (21 mmol) of 4-(cis-4-tert-butylcyclohexylamino)-5-chloro-6-(1-methylsulfinylethyl)pyrimidine (Example 26) in 100 ml of diethylene glycol dimethyl ether to which a little hydroquinone had been added was heated at 150° C. for 30 minutes. After cooling to room temperature the mixture was poured into water and extracted by stirring with dichloromethane. This left a brown oil which was extracted twice by stirring with petroleum ether. The petroleum ether phase was concentrated and the residue was purified with chromatography on silica gel, to give 1.1 g (17.8% of theory) of colorless solid.

1. temperatureAfter cooling to room temperature the mixture
2. extractionextracted
3. waitThis left a brown oil which
4. extractionwas extracted twice
5. stirringby stirring with petroleum ether
6. concentrationThe petroleum ether phase was concentrated
7. customthe residue was purified with chromatography on silica gel
8. customto give 1.1 g (17.8% of theory) of colorless solid