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负载于三唑基官能化超交联聚合物上的钯作为用于铃木-宫浦偶联反应的可回收催化剂。

Palladium supported on triazolyl-functionalized hypercrosslinked polymers as a recyclable catalyst for Suzuki-Miyaura coupling reactions.

作者信息

Liu Cijie, Zheng Lijuan, Xiang Dexuan, Liu Shasha, Xu Wei, Luo Qionglin, Shu You, Ouyang Yuejun, Lin Hongwei

机构信息

Hunan Engineering Laboratory for Preparation Technology of Polyvinyl Alcohol (PVA) Fiber Material, Key Laboratory of Research and Utilization of Ethnomedicinal Plant Resources of Hunan Province, Huaihua University Huaihua 418000 China

出版信息

RSC Adv. 2020 May 1;10(29):17123-17128. doi: 10.1039/d0ra01190h. eCollection 2020 Apr 29.

Abstract

A novel hypercrosslinked polymers-palladium (HCPs-Pd) catalyst was successfully prepared the external cross-linking reactions of substituted 1,2,3-triazoles with benzene and formaldehyde dimethyl acetal. The preparation of HCPs-Pd has the advantages of low cost, mild conditions, simple procedure, easy separation and high yield. The catalyst structure and composition were characterized by N sorption, TGA, FT-IR, SEM, EDX, TEM, XPS and ICP-AES. The HCPs were found to possess high specific surface area, large micropore volume, chemical and thermal stability, low skeletal bone density and good dispersion for palladium chloride. The catalytic performance of HCPs-Pd was evaluated in Suzuki-Miyaura coupling reactions. The results show that HCPs-Pd is a highly active catalyst for the Suzuki-Miyaura coupling reaction in HO/EtOH solvent with TON numbers up to 1.66 × 10. The yield of biaryls reached 99%. In this reaction, the catalyst was easily recovered and reused six times without a significant decrease in activity.

摘要

通过取代的1,2,3 - 三唑与苯和甲醛二甲基缩醛的外部交联反应成功制备了一种新型的超交联聚合物 - 钯(HCPs - Pd)催化剂。HCPs - Pd的制备具有成本低、条件温和、步骤简单、易于分离和产率高的优点。通过N吸附、热重分析(TGA)、傅里叶变换红外光谱(FT - IR)、扫描电子显微镜(SEM)、能谱分析(EDX)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)和电感耦合等离子体发射光谱(ICP - AES)对催化剂的结构和组成进行了表征。发现HCPs具有高比表面积、大微孔体积、化学和热稳定性、低骨架密度以及对氯化钯的良好分散性。在铃木 - 宫浦(Suzuki - Miyaura)偶联反应中评估了HCPs - Pd的催化性能。结果表明,HCPs - Pd在HO/EtOH溶剂中是铃木 - 宫浦偶联反应的高活性催化剂,其TON数高达1.66×10。联芳基的产率达到99%。在该反应中,催化剂易于回收并重复使用六次,活性没有明显下降。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fd2e/9053621/67adac29d773/d0ra01190h-f1.jpg

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