医药中间体对氯溴苯的合成新方法

A New Method for Synthesis of Pharmaceutical Intermediate p-Bromochlorobenzene

以氯苯为原料,溴素为溴源,铁粉为催化剂,对在超声波作用下合成对氯溴苯的反应进行了研究,通过单因素实验考察了反应时间、反应温度、超声波频率、催化剂用量和物料配比等因素对反应产率的影响,得到了较佳的工艺条件,并与传统方法进行了对比试验。较佳反应条件是:以等物质的量的氯苯和溴作为反应物,催化剂的物质的量是反应物的物质的量的1/10,滴溴时间20 min,继续震荡时间10 min,反应温度20℃,超声频率40 kHz,对氯溴苯产率为53.44%。

Chlorobenzene as raw material,bromine as bromo source,iron powder as catalyst.The synthesis reaction of p-Bromochlorobenzene under ultrasonic irradiation is studied.Through the single factor experiment,factors influencing the product yield are discussed:such as reaction time,reaction temperature,ultrasonic frequency,amount of catalyst and molratio of raw material.The better conditions for this reaction has been established.Meanwhile,this reaction method has carried on the contrast experiment with traditional method.The better conditions for this reaction are investigated.Using the equal amount of substance of chlorobenzene and bromine as reactants,the amount of catalyst material is one tenth of the amount of reactant material.Bromine dripping time is 20 min,then continue to shock 10 min.Reaction temperature is 20℃.Ultrasonic frequency is 40 kHz.The yield of p-Bromochlorobenzene is 53.44%.