反应详情

温度

130 °C

A mixture of methyl 2-bromo-5-methylbenzoate (0.629 g, 2.747 mmol), 2-(tributylstannyl)pyridine (1.32 g, 3.585 mmol), CsF (0.834 g, 5.494 mmol), Pd(PPh3)4 (0.4 g, 0.27 mmol), and CuI (0.105 g, 0.549 mmol) in DMF (20 mL) was degassed for 10 min and then heated in the microwave reactor for 30 min at 130° C. The mixture was cooled and the solvent was removed in vacuo. The crude was dissolved with EtOAc and then washed with saturated NaHCO3 and dried over Na2SO4. The solvent was removed in vacuo to obtain the crude, which was purified by silica gel to obtain the title compound. ESI-MS (m/z): 228 [M+1]+.

1. customwas degassed for 10 min
2. temperatureThe mixture was cooled
3. customthe solvent was removed in vacuo
4. dissolutionThe crude was dissolved with EtOAc
5. washwashed with saturated NaHCO3
6. dry with materialdried over Na2SO4
7. customThe solvent was removed in vacuo
8. customto obtain the crude, which
9. customwas purified by silica gel