反応 #288
ord-77e8bb12d76a4a1d94f2c62d1d96fda1
反応方程式
溶媒
反応条件
実験手順
diacetoxypalladium (2.322 g, 10.34 mmol) was added to a stirred suspension of 4-bromo-1-methoxy-2-nitrobenzene (30 g, 129.29 mmol), 1-(piperazin-1-yl)ethanone (16.57 g, 129.29 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (8.98 g, 15.52 mmol) and cesium carbonate (84 g, 258.59 mmol) dissolved in dioxane (300 mL) , degased and under argon. The resulting suspension was stirred at 120 °C for 2 hours.At 25°C, the mixture was filtered and adsorbed on silica gel .The crude product was purified by flash chromatography on silica gel eluting with 1 to 5% methanol in ethyle acetate. The solvent was evaporated to dryness to afford 1-(4-(4-methoxy-3-nitrophenyl)piperazin-1-yl)ethanone (31.0 g, 86 %) as a orange solid.