368 resultados para FACILE SONOCHEMICAL SYNTHESIS

em Indian Institute of Science - Bangalore - Índia


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Enantiospecific synthesis of bio-active butenolide (+)-iso-cladospolide B from D-(-)-tartaric acid in a short synthetic sequence is presented. Pivotal reaction sequence includes cross metathesis of an alkene and Wittig olefination. (C) 2010 Elsevier Ltd. All rights reserved.

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Well uniform microspheres of phase pure Covellite were synthesized through a simple hydrothermal approach using poly vinyl pyrrolidone (PVP) as surfactant. The micro-spheres were constituted of numerous self-organized knitted nano-ribbons of similar to 30 nm thickness. The effect of conc. PVP in the hydrothermal precursor solution on the product morphology was investigated. Based on the out-coming product micro-architecture a growth mechanism was proposed which emphasized bubbled nucleation inside the hydrothermal reactor. In a comparative study on linear optical properties, enhancement of luminescent intensity was observed for nano-ribbon clung microspheres rather than that of agglomerates of distorted particles, which may be attributed to better crystallinity as well as reduced surface defects and ionic vacancies for ribbon-like nano-structures.

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Nanocrystalline Ce1-xFexO2-delta (0 <= x <= 0.45) and Ce0.65Fe0.33Pd0.02O2-delta of similar to 4 nm sizes were synthesized by a sonochemical method using diethyletriamine (DETA) as a complexing agent. Compounds were characterized by powder X-ray diffraction (XRD), X-ray photo-electron spectroscopy (XPS) and transmission electron microscopy (TEM). Ce1-xFexO2-delta (0 <= x <= 0.45) and Ce0.65Fe0.33Pd0.02O2-delta crystallize in fluorite structure where Fe is in +3, Ce is in +4 and Pd is in +2 oxidation state. Due to substitution of smaller Fe3+ ion in CeO2, lattice oxygen is activated and 33% Fe substituted CeO2 i.e. Ce0.67Fe0.33O1.835 reversibly releases 0.31O] up to 600 degrees C which is higher or comparable to the oxygen storage capacity of CeO2-ZrO2 based solid solutions (Catal. Today 2002, 74, 225-234). Due to interaction of redox potentials of Pd2+/0(0.89 V) and Fe3+/2+ (0.77 V) with Ce4+/3+ (1.61 V), Pd ion accelerates the electron transfer from Fe2+ to Ce4+ in Ce0.65Fe0.33Pd0.02O1.815, making it a high oxygen storage material as well as a highly active catalyst for CO oxidation and water gas shift reaction. The activation energy for CO oxidation with Ce0.65Fe0.33Pd0.02O1.815 is found to be as low as 38 kJ mol(-1). Ce0.67Fe0.33O1.835 and Ce0.65Fe0.33Pd0.02O1.815 have also shown high activity for the water gas shift reaction. CO conversion to CO2 is 100% H-2 specific with these catalysts and conversion rate was found to be as high 27.2 mu moles g(-1) s(-1) and the activation energy was found to be 46.4 kJ mol(-1) for Ce0.65Fe0.33Pd0.02O1.815.

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Mesoporous MnO2 samples with average pore-size in the range of 2-20 nm are synthesized in sonochemical method from KMnO4 by using a tri-block copolymer, namely, poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (P123) as a soft template as well as a reducing agent. The MnO2 samples are found to be poorly crystalline. On increasing the amplitude of sonication, a change in the morphology of MnO2 from nanoparticles to nanorods and also change in porosity are observed. A high BET surface area of 245 m(2) g(-1) is achieved for MnO2 sample. The MnO2 samples are subjected to electrochemical capacitance studies by cyclic voltammetry (CV) and galvanostatic charge-discharge cycling in 0.1 M aqueous Ca(NO3)(2) electrolyte. A maximum specific capacitance (SC) of 265 Fg(-1) is obtained for the MnO2 sample synthesized in sonochemical method using an amplitude of 30 mu m. The MnO2 samples also possess good electrochemical stability due to their favourable porous structure and high surface area. (C) 2012 Elsevier B.V. All rights reserved.

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Doping of TiO2 with a suitable metal ion where dopant redox potential couples with that of titanium (Ti4+) and act as catalyst for additional reduction of Ti4+ to Ti2+ (Ti4+ -> Ti3+ -> Ti2+) is envisaged here to enhance lithium storage even higher than one Li/TiO2. Accordingly, 10 atom% Pt ion substituted TiO2, Ti0.9Pt0.1O2 nanocrystallites was synthesized by sonochemical method using diethylenetriamine (DETA) as complexing agent. Powder X-ray diffraction pattern (XRD), Rietveld refinement and TEM study reveals that Ti0.9Pt0.1O2 nanocrystallites of similar to 4 nm size crystallize in anatase structure. X-ray photo-electron spectroscopy (XPS) study confirms that and both Ti and Pt are in 4+ oxidation state. Due to Pt4+ ion substitution in TiO2, reducibility of TiO2 was enhanced and Ti4+ was reduced up to Ti2+ state via coupling of Pt states (Pt4+/Pt2+/Pt-0) with Ti states (Ti4+/Ti3+/Ti2+). Galvanostatic cycling of Ti0.9Pt0.1O2 against lithium showed very high capacity of 430 mAhg(-1) or exchange of similar to 1.5Li/Ti0.9Pt0.1O2. (C) 2012 The Electrochemical Society. DOI: 10.1149/2.029208jes] All rights reserved.

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We report a simple hydrothermal synthesis of highly reproducible carbon nanoparticles in a size range between 2 and 7 nmfroma single precursor sucrose without either surface passivating agents or acids and bases. The carbon nanoparticles can be used as white light phosphors, especially for ultraviolet light emitting diodes and metal-free catalyst for the reduction of nitrophenol.

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Lithium sodium titanate insertion-type anode has been synthesized by classical solid-state (dry) and an alternate solution-assisted (wet) sonochemical synthesis routes. Successful synthesis of the target compound has been realized using simple Na- and Li-hydroxide salts along with titania. In contrast to the previous reports, these energy-savvy synthesis routes can yield the final product by calcination at 650 -750 degrees C for limited duration of 1-10 h. Owing to the restricted calcination duration (dry route for 1-2 h and wet route for 1-5 h), they yield homogeneous nanoscale lithium sodium titanate particles. Sono-chemical synthesis reduces the lithium sodium titanate particle size down to 80-100 nm vis-a-vis solid-state method delivering larger (200-500 nm) particles. Independent of the synthetic methods, the end products deliver reversible electrochemical performance with reversible capacity exceeding 80 mAh.g(-1) acting as a 1.3 V anode for Li-ion batteries. (C) 2015 Elsevier B.V. All rights reserved.

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Retaining the morphology of gallium oxide nanostructures during structural transformations or after doping with lanthanide ions is not facile. Here we report on the sonochemical synthesis of nearly monodisperse similar to 550 nm long nano-spindles of undoped and La-doped alpha-GaOOH. The transformation of as-prepared undoped and La-doped alpha-GaOOH powders into the corresponding undoped and La-doped Ga2O3 phases (alpha and beta) was achieved by carrying out controlled annealing at elevated temperatures under optimized conditions. The formation of gallium oxide nano-spindles is explained by invoking the phenomenon of oriented attachment, as amply supported by electron microscopy. Interestingly, the morphology of the gallium oxide nano-spindles remained conserved even after doping them with more than 1.4 at% of La3+ ions. Such robust structural stability could be attributed to the oriented attachment-type growth observed in the nano-spindles. The as-prepared samples and the corresponding annealed ones were thoroughly characterized by powder X-ray diffraction (PXRD), electron microscopy (SEM, TEM, and STEM-EDS) and X-ray photoelectron spectroscopy (XPS). Finally, photoluminescence from the single-crystalline undoped and La-doped beta-Ga2O3 was explored.

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Silver nanoparticles (AgNPs) find use in different biomedical applications including wound healing and cancer. We propose that the efficacy of the nanoparticles can be further augmented by using these particles for gene delivery applications. The objective of this work was to engineer biofunctionalized stable AgNPs with good DNA binding ability for efficient transfection and minimal toxicity. Herein, we report on the one-pot facile green synthesis of polyethylene glycol (PEG) stabilized chitosan-g-polyacrylamide modified AgNPs. The size of the PEG stabilized AgNPs was 38 +/- 4 nm with a tighter size distribution compared to the unstabilized nanoparticles which showed bimodal distribution of particle sizes of 68 +/- 5 nm and 7 +/- 4 nm. To enhance the efficiency of gene transfection, the Arg-Gly-Asp-Ser (RGDS) peptide was immobilized on the silver nanoparticles. The transfection efficiency of AgNPs increased significantly after immobilization of the RGDS peptide reaching up to 42 +/- 4% and 30 +/- 3% in HeLa and A549 cells, respectively, and significantly higher than 34 +/- 3% and 23 +/- 2%, respectively, with the use of polyethyleneimine (25 kDa). These nanoparticles were found to induce minimal cellular toxicity. Differences in cellular uptake mechanisms with RGDS immobilization resulting in improved efficiency are elucidated. This study presents biofunctionalized AgNPs for potential use as efficient nonviral carriers for gene delivery with minimal cytotoxicity toward augmenting the therapeutic efficacy of AgNPs used in different biomedical products.

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Stable 1,2-dihydroisoquinolines have been synthesized by an amide catalysed novel isomerization reaction of 5,6-dihydroisoquinolines.

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Herein, we report a simple and efficient methodology for the synthesis of beta-amino disulfides by regioselective ring opening of sulfamidates with benzyltriethylammonium tetrathiomolybdate [BnNEt3](2)MoS4. Stability and reactivity of different protecting groups under the reaction conditions have been discussed. This methodology has also been extended to serine and threonine derived sulfamidates to furnish cystine and 3,3'-dimethyl cystine derivatives.

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Effect of sonochemical irradiation on the conversion of 2-alkoxytetrahydrofurans to γ-butyro-1actores by Jones reagent, and its extension to the highly stereoselective synthesis of quercus lactone a, is reported.

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A facile, one-pot synthesis of thio and selenourea derivatives from amines using tetrathiomolybdate 1 and tetraseleno-tungstate 2 as sulfur and selenium transfer reagents, respectively, is reported. The compounds were tested for their activity as urease inhibitors and some of the compounds showed potent activity in the nanomolar range towards jack bean urease. (C) 2007 Elsevier Ltd. All rights reserved.

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An interesting sulfur transfer reaction with benzyltriethylammonium tetrathiomolybdate has been used efficiently for the synthesis of macrocyclic disulfides. This methodology has been extended to a high-yield synthesis of ''redox-switched'' crown ethers which have potential application for selective ion transport across liquid membranes.