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电喷雾萃取电离质谱在线监测 Friedl?nder 缩合反应
引用本文:杨小丽,谢宗波,周鹏,艾锋,乐长高.电喷雾萃取电离质谱在线监测 Friedl?nder 缩合反应[J].化学通报,2018,81(5):445-449.
作者姓名:杨小丽  谢宗波  周鹏  艾锋  乐长高
作者单位:东华理工大学应用化学系;东华理工大学江西省质谱科学与仪器2011协同创新中心
基金项目:国家自然科学基金 (Nos. 21465002, 21520102007), 江西省优势科技创新团队建设计划项目(No. 20152BCB24003), 长江学者和创新团队发展计划 (No. IRT13054).
摘    要: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。

关 键 词:电喷雾萃取电离质谱  在线监测  反应机理  Friedl?nder  缩合反应
收稿时间:2017/7/10 0:00:00
修稿时间:2017/9/30 0:00:00

Online Monitoring of Friedl?nder Reaction Using Extractive Electrospray Ionization Tandem Mass Spectrometry
Yang Xiao Li,Xie Zongbo,Zhou Peng,Ai Feng and Le Zhanggao.Online Monitoring of Friedl?nder Reaction Using Extractive Electrospray Ionization Tandem Mass Spectrometry[J].Chemistry,2018,81(5):445-449.
Authors:Yang Xiao Li  Xie Zongbo  Zhou Peng  Ai Feng and Le Zhanggao
Abstract: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 about 2-Aminoacetophenone and acetylacetone under the condition of 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. and the reaction mechanism was deduced.
Keywords:Electrospray Ionization  Online Monitoring  Reaction Mechanism  Friedl?nder Condensation Reaction
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