PIFA-Mediated Oxidative Cyclization of 1-Carbamoyl-1-oximylcycloalkanes: Synthesis of Spiro-Fused Pyrazolin-5-one N-Oxides

convenient and efficient synthesis of spiro-fused pyrazolin-5-one N-oxides starting from readily available 1-carbamoyl-1-oximylcycloalkanes is developed. This general protocol features a novel and facile way for access to the five-membered azaheterocycles by formation of a new N-N single bond. The key cyclization step utilizes the formation of an N-oxonitrenium intermediate, mediated by the hypervalent iodine reagent PIFA, and its subsequent intramolecular trapping by the amide moiety under rather mild experimental conditions.

High-density gold nanoparticles supported on a [Ru(bpy)(3)](2+)-doped silica/Fe3O4 nanocomposite: Facile preparation, magnetically induced immobilization, and applications in ECL detection

A large-scale process combined sonication with self-assembly techniques for the preparation of high-density gold nanoparticles supported on a [Ru(bpy)(3)](2+)-doped silica/Fe3O4 nanocomposite (GNRSF) is provided. The obtained hybrid nanomaterials containing Fe3O4 spheres have high saturation magnetization, which leads to their effective immobilization on the surface of an ITO electrode through simple manipulation by an external magnetic field (without the need of a special immobilization apparatus). Furthermore, this hybrid nanomaterial film exhibits a good and very stable electrochemiluminescence (ECL) behavior, which gives a linear response for tripropylamine (TPA) concentrations between 5 mu m and 0.21 mM, with a detection limit in the micromolar range. The sensitivity of this ECL sensor can be easily controlled by the amount of [Ru(bpy)(3)](2+) immobilized on the hybrid nanomaterials (that is, varying the amount of [Ru(bpy)(3)](2+) during GNRSF synthesis).

[4+2] Annulation - Convenient Synthesis of Substituted Dihydropyranones in Aqueous Media

A facile and convenient synthesis of dihydropyranones has been developed by a formal [4+2] annulation of readily available alpha-acetyl ketene S,S-acetals with various aldehydes, involving a tandem aldol reaction and conjugate addition-elimination reaction, in the presence of NaOH in water.

Convenient Synthesis of Substituted Quinoxalines and 2H-Benzo[b][1,4]oxazines in Water

A facile and convenient synthesis method has been developed for substituted quinoxalines and 2H-benzo[b][1,4]oxazines from the reactions of alpha-bromoketones with benzene-1,2-diamine and 2-aminophenol, respectively, which were catalyzed by tetrabutyl ammonium bromide (TBAB) in aqueous basic media.

Controlled synthesis of nanoporous Au microsheet via surfactant emulsion template

A facile and wet-chemical approach was employed to control synthesis of self-organizing, hyperbranched nanoporous Au microsheet with high quality in bulk quantity. This method produced nanoporous Au microsheets with a thickness of 7-15 nm. The microsheets were composed of irregularly interconnected planar Au nanoplates with interstices, i.e. nanopores of 10-50 nm. And the nanoporous Au microsheets were enveloped in 10-30 nm thick polyaniline (PANI) sheaths. The morphology of the nanostructured Au composites could also be easily tuned by changing the concentration of aniline and chlorauric acid. The dendritic and epitaxial growth of nanoporous Au microsheet was believed as the diffusion-limited process confined in the lamellar emulsion phase through self-assembly of aniline and dodecylsulfate. The solution reaction proceeded at a mild condition (room temperature and aqueous solutions), and less toxic reagents were employed instead of extreme toxic and corrosive chemicals.

One-pot, high-yield synthesis of size-controlled gold particles with narrow size distribution

Here, we first report a facile one-step one-phase synthetic route to achieve size-controlled gold micro/nanoparticles with narrow size distribution by using o-diaminobenzene as a reducing agent in the presence of poly(N-vinyl-2-pyrrolidone) via a simple wet-chemical approach. All experimental data including that from scanning-electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and X-ray diffraction techniques indicates that the gold micro/nanoparticles with a narrow size distribution were produced in high yield (similar to 100%).

Y2O3 : Eu3+ microspheres: Solvothermal synthesis and luminescence properties

Y2O3 : Eu3+ microspheres, with an average diameter of 3 mu m, were successfully prepared through a large-scale and facile solvothermal method followed by a subsequent heat treatment. X-ray diffraction, Fourier transform infrared spectroscopy, energy-dispersive X-ray spectra, thermogravimetric and differential thermal analysis, inductive coupled plasma atomic absorption spectrometric analysis, scanning electron microscopy, transmission electron microscopy, photoluminescence spectra, as well kinetic decays, and cathodoluminescence spectra were used to characterize the samples. These microspheres were actually composed of randomly aggregated nanoparticles. The formation mechanisms for the Y2O3 : Eu3+ microspheres have been proposed on an isotropic growth mechanism. The Y2O3 : Eu3+ microspheres show a strong red emission corresponding to D-5(0) -> F-7(2) transition (610 nm) of Eu3+ under ultraviolet excitation (259 nm) and low-voltage electron beams excitation (1-5 kV), which have potential applications in fluorescent lamps and field emission displays.

Highly uniform and monodisperse beta-NaYF4 : Ln(3+) (Ln = Eu, Tb, Yb/Er, and Yb/Tm) hexagonal microprism crystals: Hydrothermal synthesis and luminescent properties

beta-NaYF4:Ln(3+) (Ln = Eu, Tb, Yb/Er, and Yb/Tm) hexagonal microprisms with remarkably uniform morphology and size have been synthesized via a facile hydrothermal route. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and photoluminescence (PL) spectra as well as kinetic decays were used to characterize the samples. It is found that sodium citrate as a shape modifier introduced into the reaction system plays a critical role in the shape evolution of the final products. Furthermore, the shape and size of the products can be further manipulated by adjusting the molar ratio of citrate/RE3+ (RE represents the total amount of Y3+ and the doped rare earth elements such as Eu3+, Tb3+, Yb3+/Er3+, or Yb3+/Tm3+). Under the excitation of 397 nm ultraviolet light, NaYF4:xEu(3+) (x = 1.5, 5%) shows the emission lines of Eu3+ corresponding to D-5(0-3) -> F-7(J) (J = 0-4) transitions from 400 to 700 nm (whole visible spectral region) with different intensity, resulting in yellow and red down-conversion (DC) light emissions, respectively.

Hydrothermal synthesis of SrCO3 : Eu3+/Tb3+ microneedles and their luminescence properties

SrCO3:Eu3+ /Tb3+ microneedles that grow along the a-axis were successfully prepared through a large-scale and facile hydrothermal method without any template and further annealing treatment. X-ray diffraction (XRD), scanning electron microscopy (SEM), and photoluminescence (PL) spectra as well kinetic decays, were used to characterize the samples. The preferential growth along a-axis for SrCO3:Eu3+/Tb3+ microneedles has been proposed through analysis of the XRD patterns of samples obtained at different hydrothermal treatment time. Under ultraviolet excitation, the SrCO3:Eu3+ and SrCO3:Tb3+ microncedle samples show a strong red and green emission corresponding to the D-5(0)-F-7(j) (J = 1, 2, 3, 4) transitions of Eu3+ and the D-5(4)-(7) F-j (J = 6, 5, 4, 3) transitions of Tb3+, respectively, which have potential applications in lighting fields.

One-step synthesis of palladium/SBA-15 nanocomposites and its catalytic application

Well-dispersed palladium nanoparticles in mesoporous SBA- 15 SiO2 were prepared in a facile one-step approach during sol-gel route under reductive atmosphere. X-ray diffraction (XRD) results indicate that as-synthesized nanocomposites basically remain ordered two-dimensional hexagonal mesostructure while transmission electron microscopy (TEM) study exhibits a well dispersion of palladium nanoparticles within the mesoporous SBA-15 channels. The size of Pd nanoparticles is approximately in the range of 5-10nm. However, the resulting nanocomposites exhibit a highly catalytic activity and reused ability at least after five recycles without ligand in air for both the Suzuki and Heck coupling reactions.

Sonochemical synthesis and luminescence properties of single-crystalline BaF2:Eu3+ nanospheres

BaF2 nanocrystals doped with 5.0 mol% Eu3+ has been successfully synthesized via a facile, quick and efficient ultrasonic solution route employing the reactions between Ba(NO3)(2), Eu(NO3)(3) and KBF4 under ambient conditions. The product was characterized via X-ray powder diffraction (XRD), scanning electron micrographs (SEM), transmission electron microscopy (TEM), high-resolution transmission electron micrographs (HRTEM), selected area electron diffraction (SAED) and photoluminescence (PL) spectra. The ultrasonic irradiation has a strong effect on the morphology of the BaF2:Eu3+ particles. The caddice-sphere-like particles with an average diameter of 250 nm could be obtained with ultrasonic irradiation, whereas only olive-like particles were produced without ultrasonic irradiation. The results of XRD indicate that the obtained BaF2:Eu3+ nanospheres crystallized well with a cubic structure. The PL spectrum shows that the BaF2:Eu3+ nanospheres has the characteristic emission of Eu3+ D-5(0)-F-7(J) (J = 1-4) transitions, with the magnetic dipole D-5(0)-F-7(1) allowed transition (590 nm) being the most prominent emission line.

Templated synthesis of composite rings using core-shell toroids

In difference to compact objects of a similar size, toroidal structures have some distinguishing properties that originate from their open inner cavity and closed circuit. Here, a general facile methodology is developed to prepare composite rings with varied compositions on a large scale by using core-shell toroids assembled from tri-block copolymers of poly(4-vinyl pyridine) (PVP)/polystyrene (PS)/PVP. Taking advantage of the complexation ability of the PVP shell, varied components that range from polymers, inorganic materials, metals and their compounds, as well as pre-formed nanoparticles are introduced to the toroidal structures to form composite nanostructures. Metal ions can be adsorbed by PVP through complexation. After in situ reduction, a large number of metal-based functional materials can be prepared. PVP is alkaline, and thus capable of catalyzing the sol-gel process to generate an inorganic shell. Furthermore, pre-formed nanoparticles can also be absorbed by the shell through specific interactions. The PS core is not infiltrative during synthesis, and hollow rings can be derived after the polymer templates are removed.

Efficient one-pot synthesis of highly substituted pyridin-2(1H)-ones via the Vilsmeier-Haack reaction of 1-acetyl,1-carbamoyl cyclopropanes

A facile and efficient one-pot synthesis of highly substituted pyridin-2(1H)-ones is developed via the Vilsmeier-Haack reaction of readily available 1-acetyl,1-carbamoyl cyclopropanes, and a mechanism involving sequential ring-opening, haloformylation, and intramolecular nucleophilic cyclization reactions is proposed.

Vilsmeier-Haack reactions of 2-arylamino-3-acetyl-5,6-dihydro-4H-pyrans toward the synthesis of highly substituted pyridin-2(1H)-ones

A facile and efficient one-pot synthesis of highly substituted pyridin-2(IH)-ones was developed via Vilsmeier-Haack reactions of readily available enaminones, 2-arylamino-3-acetyl-5,6-dihydro-4H-pyrans, and a mechanism involving sequential ring-opening, haloformylation, and intramolecular nucleophilic cyclization reactions is proposed.

Efficient synthesis of substituted tetrahydrothiopyrano[2,3-b]thiopyran-4,5-diones by a double annulation strategy from dialkenoylketene dithioacetals

An efficient synthetic procedure for substituted 2,3,6,7tetrahydrothiopyrano [2,3-b] thiopyran-4,5 -diones by a double annulation strategy is described. The ring systems are made in good yields from readily available dialkenoylketene dithioacetals in the presence of either sodium sulfide nonahydrate/N,N-dimethylformamide (DMF) or a sodium hydride/DMF/amine system.