MIL-101负载Pd纳米颗粒高效非均相催化苯并呋喃选择性C2位芳基化
收稿日期: 2017-10-10
修回日期: 2017-12-05
网络出版日期: 2017-12-15
基金资助
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.
Palladium Nanoparticles Supported on MIL-101 as an Efficient Heterogeneous Catalyst for Selective C2 Arylation of Benzofuran
Received date: 2017-10-10
Revised date: 2017-12-05
Online published: 2017-12-15
Supported by
Project supported by the National Natural Science Foundation of China (No. 21362047), the Social Development Project of Guizhou Province (No. QKHSYZ-2013-3061) and the Science and Technology Foundation of Guizhou Province (No. QKHJZ-2014-2175).
水热合成MIL-101,过量浸渍法吸附Pd(OAc)2,NaBH4原位还原Pd2+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N2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C2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C2位衍生物的简单、高效的合成方法.
徐缓 , 张茂元 , 黄香 , 史大斌 . MIL-101负载Pd纳米颗粒高效非均相催化苯并呋喃选择性C2位芳基化[J]. 有机化学, 2018 , 38(4) : 832 -839 . DOI: 10.6023/cjoc201710012
MIL-101 was synthesized by hydrothermal method, and Pd/MIL-101 catalyst was prepared by supporting palladium 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.
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