电喷雾萃取电离质谱在线监测Friedlnder缩合反应

Online Monitoring of Friedlnder Reaction Using Extractive Electrospray Ionization Tandem Mass Spectrometry

质谱在线监测有机化学反应能够实时捕捉反应过程中反应物、中间体、产物的信号及其变化情况,从而推测有机反应机理,并加深对反应本质的认识。本研究利用电喷雾萃取电离质谱(EESI-MS)技术在线监测草酸催化的邻氨基苯乙酮与乙酰丙酮间的Friedlnder缩合反应。在反应的不同时间点,分别捕捉到了反应物(m/z 136)、中间体(m/z 218、m/z 236)和产物(m/z 200)的准分子离子信号,并记录了它们的信号强度随反应时间的变化趋势,推测出了反应机理。

Mass Spectrometry online monitoring of organic chemical reaction can capture the signal and change of the reactants,intermediates,and products in the reaction process in real time so as to deepen the understanding of the nature of the reaction. In this study,extractive electrospray ionization tandem mass spectrometry（EESI-MS）were used to monitor Friedlander condensation reaction of 2-aminoacetophenone and acetylacetone using oxalate as a catalyst. At different time of the reaction,the molecular ion peak of reactants（m/z 136）,intermediates（m/z 236,m/z 218） and product（m/z 200） signal were captured,the changes of them in the course of the reaction with time trends were recorded,the reaction mechanism was deduced.