超声波联合紫外监测“一体化”低温合成二芳基乙二酮的实验研究

An experimental study on the"integrated"low-temperature synthesis of benzil by ultrasound and ultraviolet monitoring

为找到一种安全高效的合成二芳基乙二酮的方法,设计了将超声波与紫外可见分光光度计联用的“一体化”实验技术,包括超声波提取法与紫外联用抽提苯甲醛等芳香醛;超声波水浴法与紫外联用合成二芳基乙醇酮;以及超声波震荡法与紫外联用合成二芳基乙二酮。实验过程中通过紫外实时监测,低温下安全高效合成了一系列化合物。在使用超声波紫外联用技术合成二芳基乙二酮的基础上,探究了超声波功率、超声时间、氧化剂种类和取代基种类对目标化合物产率的影响。同时,实验辅助TLC监测反应进程,并对产物进行了紫外光谱、红外光谱和荧光光谱表征。实验研究表明超声波紫外联用技术是一种良好的制备二芳基乙二酮的方法,也可广泛应用于其他有机合成综合实验。

In order to find a safe and efficient method for the synthesis of benzil,an"integrated"experimental technique combining ultrasound and UV-vis spectrophotometer was designed,including ultrasonic extraction with UV for the extraction of aromatic alde-hydes,such as benzaldehyde;ultrasonic water bath with UV for the synthesis of benzoin;and ultrasonic shock with UV for the syn-thesis of benzil.A series of compounds were synthesized safely and efficiently at low temperature with real-time UV monitoring dur-ing the experiments.Based on the synthesis of benzil using ultrasonic UV coupling technique,the effects of ultrasonic power,ultra-sonic time,oxidant type and substituent type on the yields of target compounds were explored.Meanwhile,the experiment was assis-ted by TLC to monitor the reaction process.The products were also characterized by UV-vis,IR and fluorescence spectra.The exper-imental study demonstrated that the ultrasonic UV cascade technique was a good method for the preparation of benzil,which could also be widely applied to other organic synthesis experiments.