HypoGel负载Pd纳米催化剂制备与表征及温和条件下催化Suzuki反应(英文)  

Preparation and characterization of HypoGel-supported Pd nanocatalysts for Suzuki reaction under mild conditions

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作  者:Kin Hong Liew Wan Zurina Samad Norazzizi Nordin Poh Lee Loh Joon Ching Juan Mohd Ambar Yarmo Badrul Hisham Yahaya Rahimi M. Yusop 

机构地区:[1]School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM, Bangi, Selangor Darul Ehsan, Malaysia [2]Nanotechnolofly & Catalysis Research Centre (NANOCAT), University of Malaya, 50603 Kuala Lumpur, Malaysia [3]Kluster Perubatan Regeneratif, lnstitut Perubatan dan Pergigian Termaju, Universiti Sains Malaysia, 13200 Bertam Kepala Batas, Pulau Pinan9, Malaysia

出  处:《催化学报》2015年第5期771-777,共7页

基  金:supported by the Ministry of Higher Education Malaysia(FRGS/1/2012/ST01/UKM/02/1);Research Grant from UKM(IP-2014-070 and LAUREATE-2013-002)

摘  要:A new heterogeneous catalyst composed of Pd nanoparticles immobilized within a HypoG el resin has been prepared in the absence of any ligands using an extensive cross-linking method.This newly developed nanocatalyst was characterized by N_2 adsorption-desorption,X-ray diffraction(XRD),transmission electron microscopy(TEM),scanning electron microscopy(SEM),energy dispersive X-ray(EDX),Fourier transform infrared spectroscopy and inductively coupled plasma-mass spectrometer(ICP-MS)techniques.TEM and XRD results revealed that the Pd nanoparticles were well dispersed with diameters in the range of 4–12 nm,and an average size of about 8 nm.The cross-linked Pd catalyst demonstrated excellent catalytic activity towards the synthesis of a series of biaryl compounds by the reaction of various aryl halides(e.g.,bromides andiodides)with phenylboronic acid in the presence of tetrabutylammonium bromide.ICP-MS analysis indicated that there was only 0.25%weight loss of Pd(0.55±0.02 ppm)from the supported catalyst after the first cycle reaction.Furthermore,the catalyst showed excellent reusability(up to five uses)with consistently high levels of catalytic activity following its recovery by filtration.A new heterogeneous catalyst composed of Pd nanoparticles immobilized within a HypoGel resin has been prepared in the absence of any ligands using an extensive cross-linking method. This new-ly developed nanocatalyst was characterized by N2 adsorption-desorption, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy and inductively coupled plasma-mass spec-trometer (ICP-MS) techniques. TEM and XRD results revealed that the Pd nanoparticles were well dispersed with diameters in the range of 4–12 nm, and an average size of about 8 nm. The cross-linked Pd catalyst demonstrated excellent catalytic activity towards the synthesis of a series of biaryl compounds by the reaction of various aryl halides (e.g., bromides andiodides) with phenyl-boronic acid in the presence of tetrabutylammonium bromide. ICP-MS analysis indicated that there was only 0.25% weight loss of Pd (0.55 ± 0.02 ppm) from the supported catalyst after the first cycle reaction. Furthermore, the catalyst showed excellent reusability (up to five uses) with consistently high levels of catalytic activity following its recovery by filtration.

关 键 词:SUZUKI反应 纳米催化剂 温和条件 制备 PD 电感耦合等离子体质谱 傅里叶变换红外光谱 ICP-MS 

分 类 号:O621.251[理学—有机化学]

 

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