Leung Shee-Ann, Winkle Richard F, Wootton Robert C R, deMello Andrew J
Department of Chemistry, Imperial College London, Exhibition Road, South Kensington, London SW7 2AZ, UK.
Analyst. 2005 Jan;130(1):46-51. doi: 10.1039/b412069h. Epub 2004 Nov 22.
An extremely rapid tool for continuous flow synthetic process optimisation is described. A microfluidic reaction system operating in continuous flow is used in conjunction with confocal Raman microscopy to afford rapid molecule synthesis and product quantitation. Accordingly, the approach allows for rapid reaction optimisation within a continuous flow system. Specifically, the catalytic oxidation of isopropyl alcohol (IPA) to acetone using tetra-N-propylammonium perruthanate (TPAP)/N-methylmorpholine N-oxide (NMO) in a radial interdigitated micromixer is studied as a model reaction system. The composition of the reaction effluent can be determined with great facility and information relating to catalyst/co-oxidant ratios, catalyst turnovers and reaction endpoints extracted. Specifically, variation of catalyst and co-oxidant volumetric flow rates between 0 and 50 microL min(-1) is used to vary reactant concentrations, define reaction residence times and control product conversions between 0 and 100%. The rapid nature of the system allows chemical information to be gathered and utilised on a sub-minute timescale.
本文描述了一种用于连续流合成工艺优化的极快速工具。在连续流中运行的微流体反应系统与共聚焦拉曼显微镜结合使用，以实现快速分子合成和产物定量。因此，该方法允许在连续流系统内进行快速反应优化。具体而言，研究了在径向叉指式微混合器中使用四正丙基过钌酸铵（TPAP）/N-甲基吗啉N-氧化物（NMO）将异丙醇（IPA）催化氧化为丙酮的反应体系作为模型反应系统。可以非常方便地确定反应流出物的组成，并提取有关催化剂/共氧化剂比例、催化剂周转率和反应终点的信息。具体而言，催化剂和共氧化剂体积流速在0至50微升/分钟之间变化，以改变反应物浓度、定义反应停留时间并控制产物转化率在0至100%之间。该系统的快速特性使得能够在亚分钟时间尺度上收集和利用化学信息。
