反应详情

温度

90 °C

To the DMF (2 ml) solution of 2-(1,1-dimethylprop-2-ynyl)-4-methoxy-benzoic acid methyl ester (Compound AA3, 134 mg, 0.577 mmol) and N-(2-bromo-5-cyanophenyl)methanesulfonamide (Compound AA5, 167 mg, 1.05 eq.), copper iodide (9 mg, 0.08 eq.) and TEA (129 μl, 1.6 eq.) were added, degassed and flushed with nitrogen gas, added with dichlorobis(triphenylphosphine) palladium (20 mg, 0.05 eq.), and then degassed and flushed again with nitrogen gas. After stirring for 2 hr at 90° C., the reaction solution was added with water, extracted with ethyl acetate. The organic layer was washed with an brine and dried over magnesium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (white solid, 152 mg, 62%).

1. customdegassed
2. customflushed with nitrogen gas
3. customdegassed
4. customflushed again with nitrogen gas
5. additionthe reaction solution was added with water
6. extractionextracted with ethyl acetate
7. washThe organic layer was washed with an brine
8. dry with materialdried over magnesium sulfate
9. customThe drying agent was removed by filtration
10. customthe residues obtained
11. concentrationafter concentration under reduced pressure
12. customwere purified by silica gel column chromatography (ethyl acetate/hexane)