反应详情

In an argon-purged sealed tube, N-(2-(2-bromophenoxy)pyrimidin-5-yl)-4-phenylphthalazin-1-amine (150 mg, 319 μmol), pyridin-4-ylboronic acid (157 mg, 1.27 μmol), Pd(DPPF)Cl2 (47 mg, 64 μmol), sodium carbonate (239 μl, 478 μmol), and 1,4-dioxane (1.60 ml, 319 μmol) were added. The reaction was stirred at RT for 5 min. The tube was sealed and heated to 100° C. for 18 h. After 16 h, the reaction was cooled to RT, diluted with EtOAc and 10 mL of water. The product was extracted into EtOAc. The organic layer was washed with brine, dried over MgSO4, filtered, and concentrated. The product was purified by column chromatography on silica gel using 60:40 DCM:(90:10:1 DCM:MeOH:NH4OH). The resulting light brown solid was dissolved in 15 mL of DCM, the solvent were removed under vacuum, affording the title compound as a light brown solid. MS Calcd for C29H20N6O: [M]+=468. Found: [M+H]+=469.

1. customIn an argon-purged
2. customsealed tube
3. customThe tube was sealed
4. temperatureheated to 100° C. for 18 h
5. waitAfter 16 h
6. temperaturethe reaction was cooled to RT
7. extractionThe product was extracted into EtOAc
8. washThe organic layer was washed with brine
9. dry with materialdried over MgSO4
10. filtrationfiltered
11. concentrationconcentrated
12. customThe product was purified by column chromatography on silica gel using 60:40 DCM
13. dissolutionThe resulting light brown solid was dissolved in 15 mL of DCM
14. customthe solvent were removed under vacuum