High-Throughput Kinetic Screening of UV and Visible Light-Induced Copper-RDRP in Continuous Flow Using Inline Benchtop NMR Analysis

利用在线台式核磁共振分析对紫外光和可见光诱导的连续流动铜-RDRP反应进行高通量动力学筛选

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Abstract

Photoinduced copper-mediated reversible deactivation radical polymerization (photoinduced Cu-RDRP) is investigated through a simple automated continuous flow platform enabling rapid kinetic screening via inline NMR measurements. The effects of different molecular weight targets, monomers with various side chain functionalities, changes in solvent, and the ability to form polymer blocks were monitored in real-time. Offline samples were extracted to confirm the validity of the inline analysis (±4%) as well as size-exclusion chromatography (SEC) to show well-controlled polyacrylates (1.09 ≤ D̵ ≤ 1.28) with good end-group fidelity as demonstrated by matrix-assisted laser desorption/ionization time-of-flight (MALDI-ToF). Low energy visible light could be applied to polymerize polyacrylates using catalytic amounts of appropriate commercially available dyes giving full monomer conversion in only 20 min, signifying the efficiency of a user-friendly platform to optimize and monitor polymer synthesis under mild conditions.

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