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In situ monitoring of palladacycle-mediated carbonylation by surface-enhanced Raman spectroscopy

机译：通过表面增强拉曼光谱原位监测Palladacycle介导的羰基化

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摘要

Palladium-catalyzed carbonylation has emerged as one of the most potential approaches for the synthesis of carbonyl-containing molecules, however, the understanding remains challenging in many reactions partly because of a lack of robust monitoring methods. Herein, we report a novel surface-enhanced Raman spectroscopy (SERS) based strategy for the in situ monitoring of palladacycle-mediated carbonylation. The nanoplatforms integrated with SERS activity and reaction mediability were constructed through assembling new synthesized palladacycles (PCs) on the surface of gold nanoparticles. It was shown that, when carbon monoxide (CO) was introduced to the nanoplatform-containing system as a C1 source, palladacycle-mediated carbonylation was initiated, and the SERS spectra of the nanoplatforms changed concomitantly. With this SERS spectrum variation, the reaction mechanism could be investigated facilely, and the corresponding reaction was found to follow a pseudo-first-order kinetics rate law based on the relationship between the relative ratiometric peak intensities of I-1319/I-1338 and the reaction time. Therefore, using the proposed SERS approach, the carbonylation process could be directly monitored in situ without tedious pretreatments.
机译：钯催化的羰基化已成为合成含羰基分子的最潜在方法之一，但是，由于缺乏可靠的监测方法，因此在许多反应中仍然难以理解。在这里，我们报告了一种新颖的基于表面增强拉曼光谱（SERS）的策略，用于原位监测palladacycle介导的羰基化反应。通过在金纳米颗粒表面组装新合成的Palladacycles（PC），构建了具有SERS活性和反应介导性的纳米平台。结果表明，将一氧化碳（CO）作为C1源引入含纳米平台的系统时，启动了由Palladacycle介导的羰基化反应，纳米平台的SERS光谱随之变化。利用这种SERS光谱变化，可以轻松地研究反应机理，并且根据I-1319 / I-1338的相对比例峰强度与I-1319 / I-1338的相对比例峰强度之间的关系，发现相应的反应遵循拟一级动力学速率定律。反应时间。因此，使用建议的SERS方法，可以直接进行羰基化过程的现场监测，而无需进行繁琐的预处理。

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