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1.
A novel heterogenized organometallic catalyst was synthesized by coordinating palladium with polyvinyl alcohol‐functionalized Fe3O4@SiO2 nanospheres. This novel catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscope, field emission scanning electron microscope, dynamic light scattering, UV–vis spectroscopy, X‐ray photoelectron spectroscopy, energy dispersive X‐ray analysis, thermogravimetric analysis and inductively coupled plasma analysis. The prepared palladium nanoparticles supported on polyvinyl alcohol functionalized Fe3O4@SiO2 nanoparticles were successfully applied as a magnetically recyclable catalyst in Heck and Sonogashira coupling reactions in water. They showed remarkable activity toward aryl halides (I, Br, Cl) using very low palladium loading in excellent yields and demonstrated high TONs (mmol of product per mmol of catalyst). Also, the catalyst could be magnetically separated and reused seven times without any appreciable loss of catalytic activity.  相似文献   

2.
The preparation of Ni@Pd core–shell nanoparticles immobilized on yolk–shell Fe3O4@polyaniline composites is reported. Fe3O4 nanoclusters were first synthesized through the solvothermal method and then the SiO2 shell was coated on the Fe3O4 surface via a sol–gel process. To prepare Fe3O4@SiO2@polyaniline composites, polyvinylpyrrolidone was first grafted on to the surface of Fe3O4@SiO2 composites and subsequently polymerization of aniline was carried out via an ultrasound‐assisted in situ surface polymerization method. Selective etching of the middle SiO2 layer was then accomplished to obtain the yolk–shell Fe3O4@polyaniline composites. The approach uses polyaniline (PANI) conductive polymer as a template for the synthesis of Ni@Pd core–shell nanoparticles. The catalytic activity of the synthesized yolk–shell Fe3O4@PANI/Ni@Pd composite was investigated in the reduction of o‐nitroaniline to benzenediamine by NaBH4, which exhibited conversion of 99% in 3 min with a very low content of the catalyst. Transmission electron microscopy, X‐ray photoelectron spectroscopy, TGA, X‐ray diffraction, UV–visible, scanning electron microscopy, X‐ray energy dispersion spectroscopy and FT‐IR were employed to characterize the synthesized nanocatalyst. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

3.
Materials having both magnetic and catalytic properties have shown great potential for practical applications. Here, a reduced graphene oxide/iron oxide/silver nanohybrid (rGO/Fe3O4/Ag NH) ternary material was prepared by green synthesis of Ag on pre‐synthesized rGO/Fe3O4. The as‐prepared rGO/Fe3O4/Ag NH was characterized using Fourier transform infrared spectroscopy, X‐ray diffractometry, Raman spectroscopy, vibrating sample magnetometry, transmission electron microscopy and energy‐dispersive X‐ray spectroscopy. rGO sheets were covered with Fe3O4 (8–16 nm) and Ag (18–40 nm) nanoparticles at high densities. The mass percentages were 13.47% (rGO), 62.52% (Fe3O4) and 24.01% (Ag). rGO/Fe3O4/Ag NH exhibited superparamagnetic behavior with high saturated magnetization (29 emu g−1 at 12 kOe), and efficiently catalyzed the reduction of 4‐nitrophenol (4‐NP) with a rate constant of 0.37 min−1, comparable to those of Ag‐based nanocatalysts. The half‐life of 4‐NP in the presence of rGO/Fe3O4/Ag NH was ca 1.86 min. rGO/Fe3O4/Ag NH could be magnetically collected and reused, and retained a high conversion efficiency of 94.4% after the fourth cycle. rGO/Fe3O4/Ag NH could potentially be used as a magnetically recoverable catalyst in the reduction of 4‐NP and environmental remediation.  相似文献   

4.
Bromine source immobilized on magnetic nanoparticles functionalized with diethylenetriamine was successfully synthesized and characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, vibrating sample magnetometry, thermogravimetric analysis and X‐ray diffraction. The catalytic activity in the synthesis of 2,3‐dihydroquinazoline‐4(1H )‐one and polyhydroquinoline derivatives and in Knoevenagel condensation was studied. The bromine catalyst can be magnetically recovered and reused several times without significant loss of its catalytic activity. All products were obtained in high to excellent yields.  相似文献   

5.
The Fe3O4 magnetic particles were modified with 1,10‐phenanthroline‐5,6‐diol (Phen) and the related Mn complex (Fe3O4@Phen@Mn) synthesized as a heterogeneous catalyst to be used for the one‐pot three‐component synthesis of various tetrazoles. The catalysts were characterized by several methods, such as the elemental analysis, FT‐IR, X‐ray powder diffraction, dispersive X‐ray spectroscopy, scanning electron microscopy, transmission electron microscopy, dynamic light scattering, thermogravimetric‐differential thermal analysis, vibrating sample magnetometer and X‐ray photoelectron spectroscopy. In addition, the antioxidant and antibacterial activities of the catalyst and its Phen ligand were in vitro screened with 2,2‐diphenyl‐1‐picrylhydrazyl by free radical scavenging methods. Results showed that the synthesized compounds possess strong antioxidant activity (IC50; 0.172  ±  0.005 mg ml?1) as well as a good antibacterial potential in comparison to standards.  相似文献   

6.
In the present study, Fe3O4 nanoparticles were prepared via simple and versatile procedure. Then, a novel and green catalyst was synthesized by the immobilization of Ni on Fe3O4 nanoparticles coated with adenine. The activity of this nanostructure compound was examined for the oxidation of sulfides, oxidative coupling of thiols and synthesis of polyhydroquinolines. The prepared catalyst was characterized by Fourier transform infrared spectroscopy (FT‐IR), scanning electron microscopy (SEM), energy‐dispersive X‐ray spectroscopy (EDS), inductively coupled plasma optical emission spectroscopy (ICP‐OES), X‐ray Diffraction (XRD), thermal gravimetric analysis (TGA), and vibrating sample magnetometer (VSM) measurements. This organometallic catalyst was recovered by the assistance of an external magnetic field from the reaction mixture and reused for seven continuous cycles without noticeable change in its catalytic activity.  相似文献   

7.
A novel Cu (II) Schiff‐base complex immobilized on core‐shell magnetic Fe3O4 nanoparticles (Fe3O4@SPNC) was successfully designed and synthesized. The structural features of these nanoparticles were studied and confirmed by using various techniques including FT‐IR spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDS), vibrating sample magnetometer (VSM), X‐Ray diffraction (XRD), wavelength dispersive X‐ray spectroscopy (WDX), and inductively coupled plasma (ICP). These newly synthesized nanoparticles have been used as efficient heterogeneous catalytic system for one‐pot multicomponent synthesis of new pyrano[2,3‐b]pyridine‐3‐carboxamide derivatives. Notably, the catalyst could be easily separated from the reaction mixture by using an external magnet and reused for several successive reaction runs with no significant loss of activity or copper leaching. The present protocol benefits from a hitherto unreported MNPs‐immobilized Cu (II) Schiff‐base complex as an efficient nanocatalyst for the synthesis of newly reported derivatives of pyrano[2,3‐b]pyridine‐3‐carboxamide from one‐pot multicomponent reactions.  相似文献   

8.
In this study, dendrimer‐encapsulated Cu(Π) nanoparticles immobilized on superparamagnetic Fe3O4@SiO2 nanoparticles were prepared via a multistep‐synthesis. Then, the synthesized composite was fully characterized by various techniques such as fourier transform infrared (FT‐IR) spectroscopy, X‐ray diffraction (XRD), dynamic light scattering (DLS), UV‐vis spectroscopy, energy dispersive X‐ray analysis (EDX), thermogravimetric analysis (TGA) and vibration sample magnetometer (VSM). From the information gained by FE‐SEM and TEM studies it can be inferred that the particles are mostly spherical in shape and have an average size of 50 nm. Also, the amount of Cu is determined to be 0.51 mmol/g in the catalyst by inductively coupled plasma (ICP) analyzer. This magnetic nano‐compound has been successfully applied as a highly efficient, magnetically recoverable and stable catalyst for N‐arylation of nitrogen heterocycles with aryl halides (I, Br) and arylboronic acids without using external ligands or additives. The catalyst was also employed in a one‐pot, three‐component reaction for the efficient and green synthesis of 5‐substituted 1H‐tetrazoles using various aldehydes, hydroxylamine hydrochloride and sodium azide in water. The magnetic catalyst can be easily separated by an external magnet bar and is recycled seven times without significant loss of its activity.  相似文献   

9.
We describe the synthesis of a novel Fe3O4/amidoxime (AO)/Pd nanocatalyst by grafting of AO groups on Fe3O4 nanoparticles and subsequent deposition of Pd nanoparticles. Prior to grafting of AO, the 2‐cyanoethyl‐functionalized Fe3O4 nanoparticles prepared through combining 2‐cyanoethyltriethoxysilane and Fe3O4 were treated with hydroxylamine. The AO‐grafted Fe3O4 nanoparticles were then used as a platform for the deposition of Pd nanoparticles. The catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, scanning and transmission electron microscopies, vibrating sample magnetometry, wavelength‐ and energy‐dispersive X‐ray spectroscopies and inductively coupled plasma analysis. Fe3O4/AO/Pd is novel phosphine‐free recyclable heterogeneous catalyst for Sonogashira reactions. Interestingly, the novel catalyst could be recovered in a facile manner from the reaction mixture by applying an external magnet device and recycled seven times without any significant loss in activity. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

10.
A simple and practical strategy for the synthesis of a novel nano‐Fe3O4‐supported organocatalyst system based on 3,4‐dihydroxypyridine (Fe3O4/Py) has been developed. The prepared catalyst was characterized using Fourier transform infrared spectroscopy, transmission and scanning electron microscopies, X‐ray diffraction, vibrating sample magnetometry and energy‐dispersive X‐ray analysis. Accordingly, the Fe3O4/Py nanoparticles show a superparamagnetic property with a saturation magnetization of 61 emu g?1, indicating potential application in magnetic separation technology. Our experimental results reveal that the pyridine‐functionalized Fe3O4 nanoparticles are an efficient base catalyst for the domino condensation of various aromatic aldehydes, Meldrum's acid and 5‐methylpyrazol‐3‐amine under very mild reaction condition and in the presence of ethanol solvent. Moreover, the synthesized catalyst was used for one‐pot, three‐component condensation of aromatic aldehydes with barbituric acid and malononitrile to produce 7‐amino‐2,4‐dioxo‐5‐phenyl‐2,3,4,5‐tetrahydro‐1H‐pyrano[2,3‐d]pyrimidine‐6‐carbonitriles. All reactions are completed in short times and all products are obtained in good to excellent yields. Also, notably, the catalyst was reused five times without significant degradation in catalytic activity and performance. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

11.
Nanocellulose (NC) materials have some unique properties, which make them attractive as organic or inorganic supports for catalytic applications. Nanocatalysts with diameters of less than 100 nm are difficult to separate from the reaction mixture, therefore, magnetic nanoparticles (MNPs) were used as catalysts to overcome this problem. Fe3O4@NCs/BF0.2 as a green, bio‐based, eco‐friendly, and recyclable catalyst was synthesized and characterized using fourier‐transform infrared spectroscopy (FT‐IR), vibrating sample magnetometer (VSM), X‐ray diffraction (XRD), X‐ray fluorescence (XRF), Brunauer–Emmett–Teller (BET), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and thermal gravimetric analysis (TGA) techniques. Fe3O4@NCs/BF0.2 was employed for the synthesis of 2,3‐dihydro‐1H‐perimidine derivatives via a reaction of 1,8‐diaminonaphthalene with various aldehydes at room temperature under solvent‐free conditions. The present procedure offers several advantages including a short reaction time, excellent yields, easy separation of catalyst, and environmental friendliness.  相似文献   

12.
The heterostructured Ag nanoparticles decorated Fe3O4 Glutathione (Fe3O4‐Glu‐Ag) nanoparticles (NPs) were synthesized by sonicating glutathione (Glu) with magnetite and further surface immobilization of silver NPs on it. The ensuing magnetic nano catalyst is well characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), powder X‐ray diffraction (PXRD), thermogravimetric analysis (TGA). The prepared Fe3O4‐Glu‐Ag nanoparticles have proved to be an efficient and recyclable nanocatalyst with low catalyst loading for the reduction of nitroarenes and heteronitroarenes to respective amines in the presence of NaBH4 using water as a green solvent which could be easily separated at the end of a reaction using an external magnet and can be recycled up to 5 runs without any significant loss in catalytic activity. Gram scale study for the reduction of 4‐NP has also being carried out successfully and it has been observed that this method can serve as an efficient protocol for reduction of nitroarenes on industrial level.  相似文献   

13.
A new epoxidation catalyst has been prepared by grafting a molybdenum(VI)–oxodiperoxo complex containing an oxazine ligand, [MoO(O2)2(phox)], on chloro‐functionalized Fe3O4 nanoparticles. The synthesized heterogeneous catalyst (MoO(O2)2(phox)/Fe3O4 was characterized using powder X‐ray diffraction, scanning and transmission electron microscopies, vibrating sample magnetometry, energy‐dispersive X‐ray analysis, Fourier transform infrared spectroscopy and inductively coupled plasma atomic emission spectroscopy. The immobilized complex gave high product yields and high selectivity for epoxide compared to the corresponding homogeneous one in the epoxidation of various olefins in the presence of tert ‐butyl hydroperoxide at 95°C without any co‐solvent. Also, the heterogeneous catalyst can be recycled without a noticeable change in activity and selectivity.  相似文献   

14.
An effective one‐pot, convenient process for the synthesis of 1‐ and 5‐substituted 1H‐tetrazoles from nitriles and amines is described using1,4‐dihydroxyanthraquinone–copper(II) supported on Fe3O4@SiO2 magnetic porous nanospheres as a novel recyclable catalyst. The application of this catalyst allows the synthesis of a variety of tetrazoles in good to excellent yields. The preparation of the magnetic nanocatalyst with core–shell structure is presented by using nano‐Fe3O4 as the core, tetraethoxysilane as the silica source and poly(vinyl alcohol) as the surfactant, and then Fe3O4@SiO2 was coated with 1,4‐dihydroxyanthraquinone–copper(II) nanoparticles. The new catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, dynamic light scattering, thermogravimetric analysis, vibration sample magnetometry, X‐ray photoelectron spectroscopy, nitrogen adsorption–desorption isotherm analysis and inductively coupled plasma analysis. This new procedure offers several advantages such as short reaction times, excellent yields, operational simplicity, practicability and applicability to various substrates and absence of any tedious workup or purification. In addition, the excellent catalytic performance, thermal stability and separation of the catalyst make it a good heterogeneous system and a useful alternative to other heterogeneous catalysts. Also, the catalyst could be magnetically separated and reused six times without significant loss of catalytic activity. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

15.
Nanomagnetic bisethylferrocene‐containing ionic liquid supported on silica‐coated iron oxide (Fe3O4@SiO2@Im‐bisethylFc [HC2O4]) as a novel catalyst was designed and synthesized. The described catalyst was recycled and used without change in the time and efficiency of the condensation reaction. The Fourier transform‐infrared spectroscopy (FT‐IR), scanning electron microscopy images, X‐ray diffraction patterns, energy‐dispersive X‐ray spectroscopy, transmission electron microscope and vibrating‐sample magnetometer results confirmed the formation of Fe3O4@SiO2@Im‐bisethylFc [HC2O4] magnetic nanoparticle. The novel bis‐coumarin derivatives were identified by 1H‐NMR, 13C‐NMR, FT‐IR and CHNS analysis.  相似文献   

16.
We report a new strategy to immobilize a bromine source on the surface of magnetic Fe3O4 nanoparticles (Fe3O4 MNPs-DETA/Benzyl-Br3) leading to a magnetically recoverable catalyst, which exhibits high catalytic efficiency in oxidative coupling of thiols to the disulfides (89–98%). The Fe3O4 MNPs-DETA/Benzyl-Br3 catalyst was fabricated by anchoring 3-chloropropyltrimethoxysilane (CPTMS) on magnetic Fe3O4 nanoparticles, followed with N-benzylation and reaction with bromine in tetrachloridecarbon. The resulting nanocomposite was analyzed by a series of characterization techniques such as FT-IR, SEM, TGA, VSM and XRD. The catalyst could be recovered via magnetic attraction and could be recycled at least 5 times without appreciable decrease in activity.  相似文献   

17.
A green, novel and extremely efficient nanocatalyst was successfully synthesized by the immobilization of Ni as a transition metal on Fe3O4 nanoparticles coated with tryptophan. This nanostructured material was characterized using Fourier transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, thermogravimetric analysis, inductively coupled plasma optical emission spectroscopy, vibrating sample magnetometry and X‐ray diffraction. The prepared nanocatalyst was applied for the oxidation of sulfides, oxidative coupling of thiols and synthesis of 5‐substituted 1H‐tetrazoles. The use of non‐toxic, green and inexpensive materials, easy separation of magnetic nanoparticles from a reaction mixture using a magnetic field, efficient and one‐pot synthesis, and high yields of products are the most important advantages of this nanocatalyst.  相似文献   

18.
Urea‐based ionic liquid stabilized on silica‐coated Fe3O4 magnetic nanoparticles, {Fe3O4@SiO2@(CH2)3‐Urea‐SO3H/HCl}, as an unexceptionable and smooth releasing urea fertilizer in alkali soils was synthesized and fully characterized using Fourier transform infrared, UV–visible and energy‐dispersive X‐ray spectroscopies, X‐ray diffraction, scanning and transmission electron microscopies, atomic force microscopy and thermogravimetric analysis. The nanostructure catalyst as a novel, green and efficient catalyst was applied for the synthesis of bis(indolyl)methane derivatives via the condensation reaction between 2‐methylindole and aldehydes at room temperature under solvent‐free conditions. Also, pyrano[2,3‐d]pyrimidinone derivatives were prepared in the presence of the nanomagnetic urea‐based catalyst by the one‐pot three‐component condensation reaction of 1,3‐dimethylbarbituric acid, aldehydes and malononitrile under solvent‐free conditions at 60 °C. To the best of our knowledge, this is the first report of the synthesis of urea‐based ionic liquid stabilized on silica‐coated Fe3O4 magnetic nanoparticles. So the present work can open up a new and promising insight in the course of rational design, synthesis and applications of task‐specific fertilizer‐based nanomagnetic ionic liquids with desirable properties as unexceptionable substances for sustainable processes. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

19.
A new magnetically separable nickel catalyst (Ni(NO3)2?Imine/Thiophene‐Fe3O4@SiO2) was readily prepared and structurally characterized by Fourier transform infrared spectroscopy (FT‐IR), Scanning electron microscopy (SEM), Energy‐dispersive X‐ray spectroscopy (EDX), Vibrating sample magnetometer (VSM), X‐Ray diffraction (XRD) and Atomic absorption spectroscopy (AAS). The Ni(NO3)2?Imine/Thiophene‐Fe3O4@SiO2 exhibited efficient catalytic activity in the synthesis of 2,3‐dihydroquinazoline‐4(1H)‐ones and polyhydroquinolines. Catalysis research under water and solvent‐free conditions makes also this synthetic protocol ideal and fascinating from the environmental point of view. The catalyst can be magnetically recovered after the reaction and can be reused for many times without appreciable decrease in activity.  相似文献   

20.
Two new Fe3O4 microspheres‐supported semi‐homogeneous catalysts, namely Fe3O4‐G4‐polyaminoamido (PAMAM) dendrimers‐Pd(0) and Fe3O4‐polyethylene glycols (PEGs)‐Pd(0) were synthesized and characterized by X‐ray powder diffraction, infrared spectrum, scanning electron microscopy, transmission electron microscopy, X‐ray photoelectron spectroscopy and thermal gravimetric analysis, which can catalyze Suzuki coupling reactions. The performance of catalysts was tested for the reactions of aryl halides with phenyl boronic acid and compared with a heterogeneous catalyst Fe3O4‐(3‐aminopropyl)triethoxysilane (APTS)‐Pd(0), in which Fe3O4‐G4‐PAMAM dendrimers‐Pd(0) shows the best activity among the three catalysts. The order of the catalytic activities is Fe3O4‐G4‐PAMAM dendrimers‐Pd(0)>Fe3O4‐PEGs‐Pd(0)>Fe3O4‐APTS‐Pd(0). The catalysts can be quickly and completely recovered by simply applying a magnet of 105 mT and the efficiencies remain unaltered even after four recycles.  相似文献   

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