反应详情

温度

100 °C

In a 20-mL sealed tube was dissolved 4-(2-(4-aminophenoxy)pyridin-3-yl)-1-H-pyrazole-3-carbonitrile (0.120 g, 0.433 mmol) in t-BuOH (1.0 mL). Then 1-chloro-4-phenylphthalazine (0.104 g, 0.433 mmol) was added and the mixture was stirred at 100° C. for 3 days. The reaction was cooled to RT, concentrated and purified on a Gilson reverse phase chromatography system. The title compound was extracted into CH2Cl2, washed 1× saturated NaHCO3, 1×H2O, dried over Na2SO4, filtered through fritted funnel and concentrated. The title compound was further purified by silica gel chromatography using 10-100% EtOAc/Hexanes to afford 4-(2-(4-(4-phenylphthalazin-1-ylamino)phenoxy)pyridin-3-yl)-1-H-pyrazole-3-carbonitrile as light yellow solid. MS m/z=482 [M+1]+. Calc'd for C29H19N7O: 481.51.

1. customIn a 20-mL sealed tube
2. temperatureThe reaction was cooled to RT
3. concentrationconcentrated
4. custompurified on a Gilson reverse phase chromatography system
5. extractionThe title compound was extracted into CH2Cl2
6. washwashed 1× saturated NaHCO3, 1×H2O
7. dry with materialdried over Na2SO4
8. filtrationfiltered through fritted funnel
9. concentrationconcentrated
10. customThe title compound was further purified by silica gel chromatography