反应详情

To a solution of compound 6-chloro-N2-(3-chloro-4-methoxy-phenyl)-N4-cycloheptyl-pyrimidine-2,4-diamine (0.15 g, 0.39 mmol) in 1-butanol (5 mL) was added 4-hydroxypiperidine (0.12 g, 1.18 mmol) at 25° C. with stirring. To this triethylamine (0.43 mL, 3.15 mmol) was added dropwise and the mixture was stirred at 25° C. for 30 minutes. This was heated and refluxed for 12 hours under nitrogen atmosphere. The mixture was concentrated under vacuum, diluted with cold water (30 mL) and extracted with ethyl acetate (2×30 mL). The organic layers were collected, combined, washed with brine (30 mL), dried over anhydrous sodium sulphate, and concentrated under vacuum to give the desired compound. Yield: 23%.

1. stirringthe mixture was stirred at 25° C. for 30 minutes
2. temperatureThis was heated
3. temperaturerefluxed for 12 hours under nitrogen atmosphere
4. concentrationThe mixture was concentrated under vacuum
5. additiondiluted with cold water (30 mL)
6. extractionextracted with ethyl acetate (2×30 mL)
7. customThe organic layers were collected
8. washwashed with brine (30 mL)
9. dry with materialdried over anhydrous sodium sulphate
10. concentrationconcentrated under vacuum