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在微波辐射下 ,用Halex法合成了对氟硝基苯 ,考察了影响反应的主要因素 ,寻找出较佳的工艺条件为对氯硝基苯 10mmol,氟化钾 15mmol,以四甲基氯化铵为催化剂 ,用量为1mmol ,以二甲基亚砜为溶剂 ,用量为 5mL ,微波功率对应于所用商品微波炉“高火”档 ,辐射时间为 30min ,气相色谱分析收率为 86 .9% ,微波法的反应速率是常规加热法反应速率的 2 0倍 .在该条件下进行了放大的重复试验 ,重复性好
Under microwave irradiation, p-fluoronitrobenzene was synthesized by Halex method. The main factors affecting the reaction were investigated. The optimum conditions were found to be p-chloronitrobenzene 10 mmol, potassium fluoride 15 mmol, Ammonia was used as the catalyst in an amount of 1 mmol and dimethylsulfoxide was used as the solvent in an amount of 5 mL. The microwave power corresponds to the “high fire” range of the commercial microwave oven, and the irradiation time was 30 min. The yield of the gas chromatographic analysis was 86.9% The reaction rate of the microwave method is 20 times that of the conventional heating method, and under this condition, the amplification is repeated and the repeatability is good