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首页> 外文期刊>Chemistry: A European journal >A fast-initiating ionically tagged ruthenium complex: A robust supported pre-catalyst for batch-process and continuous-flow olefin metathesis
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A fast-initiating ionically tagged ruthenium complex: A robust supported pre-catalyst for batch-process and continuous-flow olefin metathesis

机译：快速引发的离子标记钌络合物：用于分批工艺和连续流烯烃复分解的稳健的负载型预催化剂

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摘要

In this study, a new pyridinium-tagged Ru complex was designed and anchored onto sulfonated silica, thereby forming a robust and highly active supported olefin-metathesis pre-catalyst for applications under batch and continuous-flow conditions. The involvement of an oxazine-benzylidene ligand allowed the reactivity of the formed Ru pre-catalyst to be efficiently controlled through both steric and electronic activation. The oxazine scaffold facilitated the introduction of the pyridinium tag, thereby affording the corresponding cationic pre-catalyst in good yield. Excellent activities in ring-closing (RCM), cross (CM), and enyne metathesis were observed with only 0.5mol % loading of the pre-catalyst. When this powerful pre-catalyst was immobilized onto a silica-based cationic-exchange resin, a versatile catalytically active material for batch reactions was generated that also served as fixed-bed material for flow reactors. This system could be reused at 1mol % loading to afford metathesis products in high purity with very low ruthenium contamination under batch conditions (below 5ppm). Scavenging procedures for both batch and flow processes were conducted, which led to a lowering of the ruthenium content to as little as one tenth of the original values. Tag! You're it! A pyridinium-tagged Ru complex (see figure) that was anchored to sulfonated silica formed a robust and highly active supported olefin-metathesis pre-catalyst for applications under batch and continuous-flow conditions with low ruthenium leaching.
机译：在这项研究中，设计了一种新的带有吡啶鎓标记的Ru络合物，并将其固定在磺化二氧化硅上，从而形成了一种坚固且高活性的负载型烯烃复分解预催化剂，可用于间歇和连续流动条件下。恶嗪-亚苄基配体的参与允许通过空间和电子活化来有效控制形成的Ru预催化剂的反应性。恶嗪支架促进了吡啶鎓标签的引入，从而以高收率提供了相应的阳离子预催化剂。在仅0.5mol％的预催化剂负载下，观察到在闭环（RCM），交叉（CM）和烯炔复分解中的优异活性。当这种功能强大的预催化剂固定在二氧化硅基阳离子交换树脂上时，就生成了用于批反应的通用催化活性材料，该材料也可用作流动反应器的固定床材料。该系统可以在1摩尔％的负载下重复使用，以提供高纯度的复分解产物，并且在分批条件下（低于5ppm）钌的污染极低。进行了分批处理和流动处理的清除程序，这导致钌含量降低到原始值的十分之一。标签！就是啦吡啶标记的Ru络合物（见图）固定在磺化二氧化硅上，形成了一种坚固且高活性的负载型烯烃复分解预催化剂，适用于间歇和连续流条件下的低钌浸出。

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