微波辐射法合成对硝基苯苄醚

Synthesis of 4-Nitrophenyl Benzyl Ether Under Microwave

采用微波辐射技术,以对硝基苯酚、氢氧化钠和氯化苄为原料,在N,N-二甲基甲酰胺(DMF)溶剂存在下直接合成对硝基苯苄醚;采用熔点测定和红外光谱对产物结构进行了分析和鉴定;考察了各反应物及其溶剂的摩尔比、微波辐射功率、微波辐射时间等因素对对硝基苯苄醚收率的影响。实验结果表明,微波辐射可明显促进对硝基苯苄醚的合成,在n(对硝基苯酚)∶n(氢氧化钠)∶n(氯化苄)∶n(DMF)=1∶1.2∶1.12∶10.36、微波辐射功率400 W、微波辐射时间5.0 m in的优化条件下,对硝基苯苄醚的收率可达95.5%。该方法具有反应过程和后处理简便、反应时间短、产物收率高等特点。

4-Nitrophenyl benzyl ether was synthesized from p-nitrophenol and benzyl chloride under microwave radiation, using N, N-dimethyl formamide （DMF） as solvent. Structures of products were identified by means of micro-melting point measuring instrument and IR. Effects of ratios of reactants to solvent, microwave irradiation power, and irradiation time on reaction were studied. Microwave irradiation can obviously increase yield of 4-nitrophenyl benzyl ether. Under optimal reaction conditions： n （p-nitrophenol） ： n （ sodium hydroxide） ： n （ benzyl chloride） ： n （DMF） 1 ： 1.2 ： 1.12 ： 10.36, microwave irradiation power 400 W, irradiation time 5.0 min, yield of 4-nitrophenyl benzyl ether can reach 95.5 %. The method is easy for operation and for separation of products.