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On-line SFC-UV/Vis-MS using flow selection interfaces to monitor continuous flow single and sequential stage organic reactions in supercritical carbon dioxide
The Journal of Supercritical Fluids ( IF 3.9 ) Pub Date : 2023-04-23 , DOI: 10.1016/j.supflu.2023.105957
Wei Guo , Ben Li , Haijun Chi , Zhongliang Jiang , Liu Qing Wei , Edward D. Ramsey

Two flow selection interfaces have been developed for connecting single or linked reactors with on-line SFC equipped with UV/Vis diode-array (DAD) and mass spectrometer detectors coupled in series (SFC-DAD-MS). This process analytical technology system, enabled the study of reactions performed in supercritical fluid carbon dioxide (SF-CO2). Each interface is designed to obtain on-line samples at different reaction progress points. Three single stage electrophilic annulation reactions performed in SF-CO2 using aniline, indole and pyrrole as amine reactants to synthesize N-heterocyclic products within a stirred continuous flow reaction vessel containing montmorillonite K-10 catalyst were monitored. Also, both stages of a two step synthetic procedure conducted within two connected continuous flow reaction coil systems were monitored using on-line SFC-DAD-MS. The first step involved a Knoevenagel reaction in SF-CO2 that provided a continuous feed to perform a second stage acetylation reaction. Use of on-line SFC-DAD-MS enabled early detection and characterization of unexpected by-products.



中文翻译:

使用流量选择界面的在线 SFC-UV/Vis-MS 监测超临界二氧化碳中连续流动的单级和连续级有机反应

已经开发了两个流量选择接口,用于将单个或连接的反应器与配备有 UV/Vis 二极管阵列 (DAD) 和串联耦合的质谱检测器 (SFC-DAD-MS) 的在线 SFC 连接。该过程分析技术系统能够研究在超临界流体二氧化碳 (SF-CO 2 ) 中进行的反应。每个接口都设计用于获取不同反应进程点的在线样品。使用苯胺、吲哚和吡咯作为胺反应物在含有蒙脱石的搅拌连续流动反应容器中,在 SF-CO 2中进行三个单级亲电环化反应监测 K-10 催化剂。此外,使用在线 SFC-DAD-MS 监测在两个连接的连续流动反应盘管系统中进行的两步合成程序的两个阶段。第一步涉及 SF-CO 2中的 Knoevenagel 反应,该反应提供连续进料以进行第二阶段乙酰化反应。使用在线 SFC-DAD-MS 可以及早检测和表征意外副产品。

更新日期:2023-04-25
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