反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
diacetoxypalladium (0.116 g, 0.52 mmol) was added to a stirred mixture of 4-bromo-1-methoxy-2-nitrobenzene (1.5 g, 6.46 mmol), 1-(piperazin-1-yl)ethanone (0.829 g, 6.46 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.449 g, 0.78 mmol) and cesium carbonate (4.21 g, 12.93 mmol) dissolved in dioxane (10 mL) , degased and under argon. The resulting suspension was stirred at 120 °C for 2 hours.At 25°C, the mixture was filtered and evaporated under reduce pressure.The mixture was 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 (1.400 g, 78 %) as a orange solid.