反应详情

THF (10 mL) and 2M sodium carbonate (2 mL) were added to a mixture of 4-chloro-8-(2,6-difluorophenyl)-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one (0.34 g, 1.0 mmol, solid-supported tetrakis(triphenylphosphine)palladium(0) (0.39 g, 0.1 mmol) and 4-fluorobenzeneboronic acid (0.21 g, 1.5 mmol). The mixture was irradiated with microwave at about 150° C. for about 20 min, then filtered and the filtrate evaporated. The crude product was redissolved in ethyl acetate (10 mL) and water (10 mL). The layers were separated and the organic layer was dried over magnesium sulphate, filtered and evaporated. The crude product was purified by flash chromatography on silica gel with cyclohexane containing ethyl acetate (0 to 50%) to give the title compound (0.25 g, 63%). LC-MS m/z 396 (M+H)+, 3.55 min (ret time).

1. customThe mixture was irradiated with microwave at about 150° C. for about 20 min
2. filtrationfiltered
3. customthe filtrate evaporated
4. dissolutionThe crude product was redissolved in ethyl acetate (10 mL)
5. customThe layers were separated
6. dry with materialthe organic layer was dried over magnesium sulphate
7. filtrationfiltered
8. customevaporated
9. customThe crude product was purified by flash chromatography on silica gel with cyclohexane
10. additioncontaining ethyl acetate (0 to 50%)