MIL-101负载Pd纳米颗粒高效非均相催化苯并呋喃选择性C_2位芳基化  

Palladium Nanoparticles Supported on MIL-101 as an Efficient Heterogeneous Catalyst for Selective C_2 Arylation of Benzofuran

作　　者：徐缓[1] 张茂元 黄香 史大斌[1] Xu Huan;Zhang Maoyuan;Huang Xiang;Shi Dabin(School of Pharmaceutical Sciences, Zunyi Medical College, Zunyi 56300)

机构地区：[1]遵义医学院药学院,遵义563000

出　　处：《有机化学》2018年第4期832-839,共8页Chinese Journal of Organic Chemistry

基　　金：国家自然科学基金(No.21362047);贵州省社会发展科技攻关(No.黔科合SY[2013]3061);贵州省科学技术基金(No.黔科合J字[2014]2175)资助项目~~

摘　　要：水热合成MIL-101,过量浸渍法吸附Pd(OAc)2,Na BH4原位还原Pd^(2+)制得Pd/MIL-101催化剂.采用X-射线衍射(XRD)、X-射线光电子能谱(XPS)、扫描电镜(SEM)、电感耦合等离子体原子发射光谱(ICP)、高分辨透射电镜(HRTEM)和N_2吸/脱附实验对其结构进行表征,催化剂Pd纳米颗粒尺寸在1.5~2.5 nm之间,质量百分数为1.5%.催化实验结果表明:Pd/MIL-101对苯并呋喃C_2位芳基化有较高的催化活性,对于活性较差的溴代芳烃,也能达到中等以上的收率,催化剂循环5次后仍能保持较高的催化活性,发展了苯并呋喃C_2位衍生物的简单、高效的合成方法.MIL-101 was synthesized by hydrothermal method, and Pd/MIL-101 catalyst was prepared by supporting palla- dium nanoparticles on metal-organic frameworks MIL-101. The microstructure and features of the catalyst were characterized by X-ray diffraction （XRD）, X-ray photoelectron spectroscopy （XPS）, scanning electron microscope （SEM）, inductive coupled plasma （ICP）, high resolution transmission electron microscopy （HRTEM） and N2 adsorption, respectively. The experimental results reveal that the Pd nanoparticles on Pd/MIL-101 range from 1.5 nm to 2.5 nm, and the content of Pd nanoparticles is 1.5%. The catalytic experiments show that Pd/MIL-101 has a high catalytic activity for the C2 arylation of benzofuran. For less active aryl bromides, the reaction gave moderate yields. Moreover, the catalyst could be recycled many times. After 5 runs of catalysis, the catalyst can still maintain high reactivity. This strategy provides a simple, effective method for the synthesis of benzofuran derivatives.

关 键 词：金属有机框架 Pd纳米颗粒 非均相催化 C-H活化 苯并呋喃 

分 类 号：O621.251[理学—有机化学]