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1.
In this paper, a highly active, air‐ and moisture‐stable and easily recoverable magnetic nanoparticles tethered mesoionic carbene palladium (II) complex (MNPs‐MIC‐Pd) as nanomagnetic catalyst was successfully synthesized by a simplistic multistep synthesis under aerobic conditions using commercially available inexpensive chemicals for the first time. The synthesized MNPs‐MIC‐Pd nanomagnetic catalyst was in‐depth characterized by numerous physicochemical techniques such as FT‐IR, ICP‐AES, FESEM, EDS, TEM, p‐XRD, XPS, TGA and BET surface area analysis. The prepared MNPs‐MIC‐Pd nanomagnetic catalyst was used to catalyze the Suzuki–Miyaura and Mizoroki–Heck cross‐coupling reactions and exhibited excellent catalytic activity for various substrates under mild reaction conditions. Moreover, MNPs‐MIC‐Pd nanomagnetic catalyst could be easily and rapidly recovered by applying an external magnet. The recovered MNPs‐MIC‐Pd nanomagnetic catalyst exhibited very good catalytic activity up to ten times in Suzuki–Miyaura and five times in Mizoroki–Heck cross‐coupling reactions without considerable loss of its catalytic activity. However, MNPs‐MIC‐Pd nanomagnetic catalyst shows notable advantages such as heterogeneous nature, efficient catalytic activity, mild reaction conditions, easy magnetic work up and recyclability.  相似文献   

2.
A new bis(N ‐heterocyclic carbene) (NHC) palladium complex supported on silica coated magnetic nanoparticles (MNPs) was prepared using the reaction of synthesized Pd‐NHC complex with MNPs. The Pd‐NHC complex was prepared using the reaction of a hydroxyl‐functionalized bis‐imidazolium ionic liquid. The Pd‐NHC organometallic complex was used as a heterogeneous recyclable and active catalyst in the Suzuki‐Miyaura reaction and various aryl halides were coupled with arylboronic acids in order to synthesize diverse biaryls in good to excellent yields. The prepared catalyst was characterized by use of some different microscopic and spectroscopic techniques including elemental analysis, FT‐IR spectroscopy, diffuse reflectance UV–Vis spectrophotometery, scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM) and X‐ray diffraction (XRD). The Pd‐NHC catalyst system is a magnetic reusable catalyst and it can be separated from the reaction mixture using an external magnetic field. The catalyst was reusable in the Suzuki‐Miyaura coupling reaction at least for 6 times without significant decreasing in its catalytic activity.  相似文献   

3.
Antibody‐conjugated magnetic nanoparticles (Ab‐MNPs) have potential in pathogen detection because they allow target cells to be easily separated from complex sample matrices. However, the sensitivity and specificity of pathogen capture by Ab‐MNPs generally vary according to the types of MNPs, antibodies, and sample matrices, as well as preparation methods, including immobilization. Therefore, achieving a reproducible analysis utilizing Ab‐MNPs as a pathogen detection method requires accurate characterization of Ab‐MNP capture ability and standardization of all handling processes. In this study, we used high‐resolution CE‐single strand conformational polymorphism coupled with a stuffer‐free multiplex ligation‐dependent probe amplification system to characterize Ab‐MNPs. The capture ability of Ab‐MNPs targeting Salmonella enteritidis and nine pathogens, including S. enteritidis, was analyzed in phosphate buffer and milk. The effect of storage conditions on the stability of Ab‐MNPs was also assessed. The results showed that the stuffer‐free multiplex ligation‐dependent probe amplification system has the potential to serve as a standard characterization method for Ab‐MNPs. Moreover, the precise characterization of Ab‐MNPs facilitated robust pathogen detection in various applications.  相似文献   

4.
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   

5.
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   

6.
The preparation of an efficient heterogeneous catalyst system based on the immobilization of palladium nanoparticles on a magnetic nanoparticle core (ImmPd(0)‐MNPs) is described. The new catalytic system was characterized using transmission and scanning electron microscopies, X‐ray diffraction, energy‐dispersive X‐ray and Fourier transform infrared spectroscopies, thermogravimetric analysis, vibrating sample magnetometry and inductively coupled plasma analysis. We have demonstrated that ImmPd(0)‐MNPs is an efficient and reusable catalyst for the Suzuki–Miyaura and Sonogashira coupling reactions of various types of aryl halides in water as a green and environmentally acceptable solvent. Moreover, the reactions were carried out efficiently at room temperature. The catalyst was easily separated using an external magnet from the reaction mixture and recycled ten times without significant loss of activity.  相似文献   

7.
We report a novel catalyst system with an immobilized palladium metal‐containing magnetic nanoparticle core (ImmPd(0)‐MNPs) for the Heck reaction. ImmPd(0)‐MNPs was found to be an exceptionally mild and versatile catalyst for the Heck reaction of aryl iodides and bromides at room temperature. The catalyst was simply recovered using an external magnet from the reaction mixture and recycled six times. The results showed that the catalyst was very active and stable. Moreover, the reaction was carried out in water as a green and environmentally acceptable solvent. In terms of scope and mildness, ImmPd(0)‐MNPs is an improvement over previously reported catalysts for Heck coupling methods.  相似文献   

8.
The Fe3O4 magnetic nanoparticles (Fe3O4 MNPs) were modified with 1,10‐phenanthroline‐5,6‐diol and the relevant Co complex (Fe3O4@Phendiol@Co) synthesized as a nano‐magnetic heterogeneous catalyst to be used for the N ‐formylation of various amines at room temperature under solvent‐free conditions. Also, in order to find the better concept of the catalyst role, the N ‐formylation reaction was carried out by the use of ultrasound irradiation in the absence of the Co nano‐catalyst and the results were compared. The catalyst characterized by different methods such as the elemental analysis (CHN), ICP, FT‐IR, XRD, EDX, SEM, TEM, TG‐DTA, VSM and XPS. In addition, the antioxidant and the antibacterial activities of the Fe3O4@Phendiol@Co nano‐catalyst and its Phendiol ligand were in vitro screened by 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH) free radical scavenging and disc diffusion methods. Results showed that they possess strong antioxidant activity (IC50; 0.182 ± 0.006 mg/ml) and good antibacterial potential in comparison to standards.  相似文献   

9.
Novel Pd nanoparticles were prepared in five successive stages: 1) preparation of the Fe3O4 magnetic nanoparticles (Fe3O4 MNPs), 2) coating of Fe3O4 MNPs with SiO2 (Fe3O4@SiO2), 3) functionalization of Fe3O4@SiO2 with 3‐chloropropyltrimethoxy‐ silane (CPTMS) ligand (Fe3O4@SiO2@CPTMS), 4) further functionalization with 3,5‐diamino‐1,2,4‐triazole (DAT) ligand (Fe3O4@SiO2@CPTMS @DAT), and 5) the complexation of Fe3O4@SiO2@CPTMS@DAT with PdCl2 (Fe3O4@SiO2@CPTMS@ DAT@Pd). Then, the obtained Pd nano‐catalyst characterized by different methods such as the elemental analysis (CHN), FT‐IR, XRD, EDX, SEM, TEM, TG‐DTA and VSM. Finally, the Pd catalyst was applied for the synthesis of various 2‐imino‐3‐phenyl‐2,3‐dihydrobenzo[d]oxazol‐5‐ols.  相似文献   

10.
The synthesis of some fluorescent 2,6‐dicyano‐3,5‐disubstituted anilines using cellulose sulfuric acid (Cellulose‐SA) as an environmentally benign catalyst in H2O is described. The one‐pot reaction of 1,3‐diketone and three equiv. of malononitrile was carried out in the presence of one equiv. of a secondary amine, Cellulose‐SA as catalyst, and H2O as solvent. The photophysical properties (λAbs., λFlu.) of the synthesized compounds in CH2Cl2, MeCN, and MeOH have been measured. The emission spectra of the new compounds in the solid state are also reported.  相似文献   

11.
In this research, solvent‐assisted dispersive micro‐SPE was introduced as a simple modified technique for the determination of parabens in water and cosmetic samples. Aminopropyl‐functionalized magnetite nanoparticles (MNPs) were successfully synthesized and applied. GC with photoionization detector was used for the separation and detection of parabens. In this method, hexylacetate (15 μL) as a solvent and aminopropyl‐functionalized MNPs (5 μg) as a sorbent were added to an aqueous sample (10 mL) and then the sample was sonicated. Dispersed magnetite was collected in the bottom of the conical tube by using a strong magnet and then ACN was added as a desorption solvent. Forty microliters of this solvent was transferred into a microvial and then acetic anhydride and pyridine were added, thus derivatization was performed by acetic anhydride. After evaporation, 1 μL of derivatized sample was injected into a gas chromatograph for analysis. Several important parameters, such as kind of organic solvent, desorption solvent and volume, amount of aminopropyl‐functionalized MNPs and effect of salt addition were investigated. Under optimum conditions, the limits of detection achieved were between 50 and 300 ng/L, with RSDs (n = 5) lower than 8%. Under the optimum conditions, the enrichment factors ranged from 217 to 1253 and the extraction recoveries ranged from 10 to 62%. The recoveries were obtained for the analytes in river water and mouthwash solution and hand cream in the range of 87–103%. The advantages of proposed method are simplicity of operation, rapidity, high extraction yields, and environmental friendly character.  相似文献   

12.
A novel t hiourea dioxide‐functionalized hydroxyapatite‐encapsulated hybrid core‐shell γ‐Fe2O3@HAp‐TUD nanoparticles (MNPs) were prepared and characterized by FT‐IR, EDX, SEM, XRD, TGA and VSM analytical methods. The catalytic activity of these MNPs was evaluated through one‐pot three‐component reactions between various substituted aldehydes, malononitrile and 3‐cyano‐6‐hydroxy‐4‐methyl‐pyridin‐2(1H )‐one to afford the corresponding pyrano[2,3‐b]pyridines in high yields under mild and solvent‐free conditions. The catalyst can be easily recycled in a magnetic field and reused in five consecutive runs without significant decrease of its catalytic activity.  相似文献   

13.
The thermal stability of several commonly used crystalline matrix‐assisted ultraviolet laser desorption/ionization mass spectrometry (UV‐MALDI‐MS) matrices, 2,5‐dihydroxybenzoic acid (gentisic acid; GA), 2,4,6‐trihydroxyacetophenone (THA), α‐cyano‐4‐hydroxycinnamic acid (CHC), 3,5‐dimethoxy‐4‐hydroxycinnamic acid (sinapinic acid; SA), 9H‐pirido[3,4‐b]indole (nor‐harmane; nor‐Ho), 1‐methyl‐9H‐pirido[3,4‐b]indole (harmane; Ho), perchlorate of nor‐harmanonium ([nor‐Ho + H]+) and perchlorate of harmanonium ([Ho + H]+) was studied by heating them at their melting point and characterizing the remaining material by using different MS techniques [electron ionization mass spectrometry (EI‐MS), ultraviolet laserdesorption/ionization‐time‐of‐flight‐mass spectrometry (UV‐LDI‐TOF‐MS) and electrospray ionization‐time‐of‐flight‐mass spectrometry (ESI‐TOF‐MS)] as well as by thin layer chromatography analysis (TLC), electronic spectroscopy (UV‐absorption, fluorescence emission and excitation spectroscopy) and 1H nuclear magnetic resonance spectroscopy (1H‐NMR). In general, all compounds, except for CHC and SA, remained unchanged after fusion. CHC showed loss of CO2, yielding the trans‐/cis‐4‐hydroxyphenylacrilonitrile mixture. This mixture was unambiguously characterized by MS and 1H‐NMR spectroscopy, and its sublimation capability was demonstrated. These results explain the well‐known cluster formation, fading (vanishing) and further recovering of CHC when used as a matrix in UV‐MALDI‐MS. Commercial SA (SA 98%; trans‐SA/cis‐SA 5 : 1) showed mainly cis‐ to‐trans thermal isomerization and, with very poor yield, loss of CO2, yielding (3′,5′‐dimethoxy‐4′‐hydroxyphenyl)‐1‐ethene as the decarboxilated product. These thermal conversions would not drastically affect its behavior as a UV‐MALDI matrix as happens in the case of CHC. Complementary studies of the photochemical stability of these matrices in solid state were also conducted. Copyright © 2008 John Wiley & Sons, Ltd.  相似文献   

14.
Starch and poly(p‐dioxanone) (PPDO) are the natural and synthetic biodegradable and biocompatible polymers, respectively. Their copolymers can find extensive applications in biomedical materials. However, it is very difficult to synthesize starch‐graft‐PPDO copolymers in common organic solvents with very good solubility. In this article, well‐defined polysaccharides‐graft‐poly(p‐dioxanone) (SAn‐PPDO) copolymers were successfully synthesized via the ring‐opening polymerization of p‐dioxanone (PDO) with an acetylated starch (SA) initiator and a Sn(Oct)2 catalyst in bulk. The copolymers were characterized via Fourier transform infrared spectroscopy, 1H NMR, gel permeation chromatography, thermogravimetric analysis (TG), differential scanning calorimetry, and wide angle x‐ray diffraction. The in vitro degradation results showed that the introduction of SA segments into the backbone chains of the copolymers led to an enhancement of the degradation rate, and the degradation rate of SAn‐PPDO increased with the increase of SA wt %. Microspheres with an average volume diameter of 20 μm, which will have potential applications in controlled release of drugs, were successfully prepared by using these new copolymers. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 5344–5353, 2009  相似文献   

15.
The palladium complex of MgO‐supported melamine‐formaldehyde polymer catalyst was prepared and characterized by X‐ray diffraction (XRD) and X‐ray photoelectron spectroscopy (XPS). The preparation of Nn‐octyl‐D ‐glucamine was investigated by using this complex as the catalyst. It was found that the palladium complex of MgO‐supported melamine‐formaldehyde polymer has a good catalytic activity for the hydrogenation of n‐octylamine with D ‐glucose to produce Nn‐octyl‐D ‐glucamine. The effects of additive, solvent, temperature, hydrogen pressure, Pd content in the catalyst and the amount of catalyst on the preparation of Nn‐octyl‐D ‐glucamine have all been studied. Under the optimum experimental conditions—D ‐glucose, 37.2 mmol; n‐octylamine, 31 mmol; triethylamine, 1.0 ml; ethanol, 60 ml; temperature, 333 K; hydrogen pressure, 1.5 MPa; the amount of the catalyst (Pd content 3.55%, N/Pd molar ratio 12), 0.7 g—the highest yield of Nn‐octyl‐D ‐glucamine (57.6%) was obtained. XRD results show that melamine‐formaldehyde polymer changed the structure of MgO, and XPS results suggest that coordination bonds were formed between the hexatomic ring and metal atom, and palladium particles were immobilized on the polymer. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

16.
Thiourea dioxide was immobilized on γ‐Fe2O3@Cu3Al‐LDH magnetic nanoparticles to prepare the γ‐Fe2O3@Cu3Al‐LDH‐TUD MNPs. The structure and properties of these magnetic nanoparticles were established by FT‐IR, EDX, SEM, XRD, and hystogram of particle size analytical methods. The results obtained from these analytical methods confirmed the successful immobilization of the thiourea dioxide onto the magnetic support. The synthesized magnetic nanoparticles (MNPs) exhibited high catalytic activity in one‐pot three‐component reactions under mild and solvent‐free conditions for the synthesis of diverse ranges of dihydropyrano[3,2‐c]pyrazoles and dihydropyrano[3,2‐c]chromens. All the reactions proceeded smoothly to furnish the respective products in excellent yields. Simple isolation of the products, avoidance of harmful organic solvents, versatility of the catalyst and its easy magnetic separation and reusability with no significant loss of activity are the main advantages of the present method.  相似文献   

17.
Fe3O4@MCM‐41@Zr‐MNPs modified with piperazine is easily prepared and characterized using Fourier transform infrared spectroscopy (FT‐IR), X‐ray powder diffraction (XRD), N2 adsorption–desorption, Transmission electron microscopy (TEM), Energy‐dispersive X‐ray (EDX), Vibrating sample magnetometry (VSM) and Thermogravimetric analysis (TGA) techniques. The characterization results showed that Zr highly dispersed in the tetrahedral environment of silica framework and piperazine is successfully attached to the surface of the nanocatalyst in connection with zirconium. The prepared nanosized reagent (10–30 nm), shows excellent catalytic activity in the synthesis of tetrahydro‐4H‐chromene and pyrano[2,3‐d]pyrimidinone derivatives. All reactions are performed under mild and completely heterogeneous reactions conditions in high yields during short reaction times. On the other hand and due to its superparamagnetic nature the catalyst can be easily separated by the application of an external magnetic field and reused for several times.  相似文献   

18.
The use of bronate affinity adsorbents is a new separation method that appeared recently with great potential for specific extraction of cis‐diol‐containing compounds. In this work,a new strategy for the facile construction of boronic acid‐functionalized Fe3O4 magnetic nanoparticles (Fe3O4@FPBA MNPs) with a high capacity was described. The extraction capacity of the Fe3O4@FPBA MNPs was determined to be 66.0 ± 2.7 µmol/g for catechol and 80.6 ± 2.0 µmol/g for dopamine, being higher than that for the reported methods. The Fe3O4@FPBA MNPs were used to extract four cis‐diol drugs: caffeic acid isopropyl ester, caffic acid bornyl ester, isopropyl 3‐(3,4‐dihydroxyphenyl)‐2‐hydroxypropanoate and 3‐(3, 4‐dihydroxyphenyl)‐2‐hydroxylpropionic acid – from the spiked rabbit plasma, and the recoveries of four drugs were between 87.29 and104.37% with relative standard deviations ranging from 1.34 to 8.81%. Under the most favorable conditions, the solid‐phase extraction combined with HPLC‐UV for the analysis of four drugs in plasma could eliminate interferences from endogenous components of the biological fluids and exhibited sufficient precision and accuracy. These results showed that the prepared Fe3O4@FPBA MNPs were qualified for efficiently enriching and determining the trace cis‐diol substances from biological samples. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

19.
In this work, we have synthesized a polycation and a polyanion via a combination of oxyanion‐initiated polymerization and polymer reaction, and then developed a novel approach to prepare a controlled magnetic target gene carrier with magnetic Fe3O4 nanoparticles as core and poly(ethylene glycol) (PEG) segment as corona via layer‐by‐layer (LbL) assembly and shell‐crosslinking. Magnetic nanoparticles (MNPs) were first modified by poly[2‐(dimethylamino)ethyl methacrylate] (PDMAEMA) via radical polymerization. The resulting MNPs were used to compact deoxyribonucleic acid (DNA) through LbL assembly, involving four steps: ( 1 ) the binding of DNA to the polycation PDMAEMA on the surface of MNPs; ( 2 ) the produced particles in Step 1 with negative charge interacting with additional polycation ethoxy group end‐capped PDMAEMA (EtO‐PDMAEMA) homopolymer, leading to a positive charge surface; ( 3 ) using carboxyl group (‐COO) of poly(methacrylic acid) (PMAA) in a diblock copolymer (MePEG2000‐b‐PMAASH) as polyanion, which has partial mercapto groups (‐SH) in PMAA segment, to interact with the particles produced in Step 2; ( 4 ) the shell of the composite nanoparticle was crosslinked by oxidizing the ‐SH groups of the MePEG2000‐b‐PMAASH to form disulfide linkage (S? S). All the processes of LbL assembly were investigated by agarose gel retardation assay and zeta potential measurements. The in vitro cytotoxicity analysis proves that polyions/DNA MNPs have excellent properties and potential applications as gene carriers. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011  相似文献   

20.
Nanogels based on biocompatible, dual pH‐ and temperature‐sensitive poly(2‐(diethylamino)ethyl) methacrylate (PDEAEMA) have been successfully used as nanocontainers for the encapsulation of magnetite, Fe3O4 magnetic nanoparticles (MNPs). For this purpose, citric acid‐coated MNPs were encapsulated into previously synthesized PDEAEMA‐based nanogels using a poly(ethyleneglycol)‐based stabilizer. After the encapsulation of the magnetite MNPs, the so‐called magneto‐nanogels (MNGs) were proved to be multiresponsive on temperature, pH, and magnetic field and colloidally stable. Moreover, preliminary studies on the biocompatibility of these MNGs with cells of human peripheral blood were performed and evidenced quite tolerable biocompatibility, thus suggesting potential use in biomedical applications. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016 , 54, 1479–1494  相似文献   

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