反应详情

温度

50 °C

Ethyl 2-(2-bromo-4-fluoro-5-nitrophenyl)acetate (1.00 g, 3.27 mmol), PdCl2(PPh3)2 (115 mg, 0.16 mmol), CuI (44 mg, 0.23 mmol), and trimethylsilylacetylene (0.7 mL, 4.9 mmol) were dissolved in Et3N (5 mL). The mixture was immediately degassed by vacuum, and the flask was charged with N2. The mixture was heated overnight at 50° C. Water was added and then the solution was extracted with EtOAc (3×). The organic was washed with NH4Cl, brine and dried (MgSO4). The solvent was removed and then the residue was purified by silica gel column chromatography to obtain ethyl 2-(4-fluoro-5-nitro-2-(2-(trimethylsilyl)ethynyl)phenyl)acetate (0.66 g, 62% yield).

1. customThe mixture was immediately degassed by vacuum
2. additionthe flask was charged with N2
3. additionWater was added
4. extractionthe solution was extracted with EtOAc (3×)
5. washThe organic was washed with NH4Cl, brine
6. dry with materialdried (MgSO4)
7. customThe solvent was removed
8. customthe residue was purified by silica gel column chromatography