scholarly journals Synthesis and Characterization of New Boron Compounds Using Reaction of Diazonium Tetraphenylborate with Enaminoamides

Molecules ◽  
2022 ◽  
Vol 27 (2) ◽  
pp. 367
Author(s):  
Markéta Svobodová ◽  
Jan Svoboda ◽  
Bing-Han Li ◽  
Valerio Bertolasi ◽  
Luboš Socha ◽  
...  
Keyword(s):  
Room Temperature ◽  
15N Nmr ◽  
Boron Compounds ◽  
Reaction Conditions ◽  
X Ray ◽  
Temperature Method ◽  
Mechanism Of Reaction ◽  
Vis Spectroscopy ◽  
11B Nmr

A family of oxazaborines, diazaborinones, triazaborines, and triazaborinones was prepared by reaction of polarized ethylenes, such as β-enaminoamides, with 4-methylbenzenediazonium tetraphenylborates. The reaction conditions (stirring in CH2Cl2 at room temperature (Method A) or stirring with CH3COONa in CH2Cl2 at room temperature (Method B) or refluxing in the CH2Cl2/toluene mixture (Method C)) controlled the formation and relative content of these compounds in the reaction mixtures from one to three products. Substituted oxazaborines gradually rearranged into diazaborinones at 250 °C. The prepared compounds were characterized by 1H NMR, 13C NMR, IR, and UV–Vis spectroscopy, HRMS, or microanalysis. The structure of individual compounds was confirmed by 11B NMR, 15N NMR, 1D NOESY, and X-ray analysis. The mechanism of reaction of enaminoamides with 4-methylbenzenediazonium tetraphenylborate was proposed.

Synthesis and Characterization of Superparamagnetic Fe3O4 Nanoparticles

2013 ◽  
Vol 750-752 ◽  
pp. 340-343 ◽  
Author(s):  
De Hui Sun ◽  
Jiao Wu ◽  
Ji Lin Zhang
Keyword(s):  
Room Temperature ◽  
Thermal Method ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Xrd Pattern ◽  
X Ray ◽  
Magnetic Investigation ◽  
Average Size

We synthesized Fe3O4 nanoparticles using a solvent thermal method and characterized the morphologies, structures, surface properties, thermal stability and magnetism of the products by Field emission scanning electron microscopy (FE-SEM), Powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), thermal gravimetric analysis (TGA) and vibrating sample magnetometer (VSM). The experimental results showed that the Fe3O4 nanoparticles have a tunable average size range from 55 nm to 85 nm. Their diameters decreased with increase of precursor FeCl24H2O concentration or increase of the reaction time under other reaction conditions held constant. The XRD pattern confirmed that the Fe3O4 nanoparticles belong to cubic structure. Magnetic investigation reveals that the Fe3O4 nanoparticles have higher saturation magnetization and negligible coercivity at room temperature.

One-pot Synthesis of Pyrazolone Sulfones by Iodine-catalyzed Sulfenylation of Pyrazolones with Aryl Sulfonyl Hydrazides Followed by Oxidation in Water

2018 ◽  
Vol 15 (3) ◽  
pp. 380-387
Author(s):  
Xia Zhao ◽  
Xiaoyu Lu ◽  
Lipeng Zhang ◽  
Tianjiao Li ◽  
Kui Lu
Keyword(s):  
Double Bond ◽  
Efficient Method ◽  
Room Temperature ◽  
Sulfonyl Chloride ◽  
Antibacterial Activities ◽  
Oxidation Reactions ◽  
Reaction Conditions ◽  
One Pot ◽  
X Ray ◽  
Amide Form

Aim and Objective: Pyrazolone sulfones have been reported to exhibit herbicidal and antibacterial activities. In spite of their good bioactivities, only a few methods have been developed to prepare pyrazolone sulfones. However, the substrate scope of these methods is limited. Moreover, the direct sulfonylation of pyrazolone by aryl sulfonyl chloride failed to give pyrazolone sulfones. Thus, developing a more efficient method to synthesize pyrazolone sulfones is very important. Materials and Method: Pyrazolone, aryl sulphonyl hydrazide, iodine, p-toluenesulphonic acid and water were mixed in a sealed tube, which was heated to 100°C for 12 hours. The mixture was cooled to 0°C and m-CPBA was added in batches. The mixture was allowed to stir for 30 min at room temperature. The crude product was purified by silica gel column chromatography to afford sulfuryl pyrazolone. Results: In all cases, the sulfenylation products were formed smoothly under the optimized reaction conditions, and were then oxidized to the corresponding sulfones in good yields by 3-chloroperoxybenzoic acid (m-CPBA) in water. Single crystal X-ray analysis of pyrazolone sulfone 4aa showed that the major tautomer of pyrazolone sulfones was the amide form instead of the enol form observed for pyrazolone thioethers. Moreover, the C=N double bond isomerized to form an α,β-unsaturated C=C double bond. Conclusion: An efficient method to synthesize pyrazolone thioethers by iodine-catalyzed sulfenylation of pyrazolones with aryl sulfonyl hydrazides in water was developed. Moreover, this method was employed to synthesize pyrazolone sulfones in one-pot by subsequent sulfenylation and oxidation reactions.

scholarly journals Synthesis and characterization of Fe, Co, and Ni colloids in 2-mercaptoethanol

2020 ◽  
Vol 10 ◽  
pp. 184798042096688
Author(s):  
Galo Cárdenas-Triviño ◽  
Sergio Triviño-Matus
Keyword(s):  
Electron Microscopy ◽  
Electron Diffraction ◽  
Colloidal Dispersions ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Transmission Electron ◽  
Vis Spectroscopy ◽  
Chemical Liquid Deposition ◽  
Liquid Deposition

Metal colloids in 2-mercaptoethanol using nanoparticles (NPs) of iron (Fe), cobalt (Co), and nickel (Ni) were prepared by chemical liquid deposition method. Transmission electron microscopy, electron diffraction, UV-VIS spectroscopy, and scanning electron microscopy with electron dispersive X-ray spectroscopy characterized the resulting colloidal dispersions. The NPs exhibited sizes with ranges from 9.8 nm for Fe, 3.7 nm for Co, and 7.2 nm for Ni. The electron diffraction shows the presence of the metals in its elemental state Fe (0), Co (0), and Ni (0) and also some compounds FeO (OH), CoCo2S4, and NiNi2S4.

scholarly journals Synthesis and Characterization of Lithium-Ion Conductive LATP-LaPO4 Composites Using La2O3 Nano-Powder

Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3502
Author(s):  
Fangzhou Song ◽  
Masayoshi Uematsu ◽  
Takeshi Yabutsuka ◽  
Takeshi Yao ◽  
Shigeomi Takai
Keyword(s):  
Room Temperature ◽  
Conduction Mechanism ◽  
Lithium Ion ◽  
X Ray Diffraction ◽  
Temperature Conductivity ◽  
Room Temperature Conductivity ◽  
X Ray ◽  
Nano Powder ◽  
Powder Addition

LATP-based composite electrolytes were prepared by sintering the mixtures of LATP precursor and La2O3 nano-powder. Powder X-ray diffraction and scanning electron microscopy suggest that La2O3 can react with LATP during sintering to form fine LaPO4 particles that are dispersed in the LATP matrix. The room temperature conductivity initially increases with La2O3 nano-powder addition showing the maximum of 0.69 mS∙cm−1 at 6 wt.%, above which, conductivity decreases with the introduction of La2O3. The activation energy of conductivity is not largely varied with the La2O3 content, suggesting that the conduction mechanism is essentially preserved despite LaPO4 dispersion. In comparison with the previously reported LATP-LLTO system, although some unidentified impurity slightly reduces the conductivity maximum, the fine dispersion of LaPO4 particles can be achieved in the LATP–La2O3 system.

scholarly journals MOVPE Growth of Quaternary (Al,Ga,In)N for UV Optoelectronics

2000 ◽  
Vol 5 (S1) ◽  
pp. 412-424
Author(s):  
Jung Han ◽  
Jeffrey J. Figiel ◽  
Gary A. Petersen ◽  
Samuel M. Myers ◽  
Mary H. Crawford ◽  
...  
Keyword(s):  
Room Temperature ◽  
Rutherford Backscattering Spectrometry ◽  
Optoelectronic Devices ◽  
Lattice Parameter ◽  
X Ray Diffraction ◽  
X Ray ◽  
Peak Energy ◽  
Movpe Growth ◽  
Pl Emission

We report the growth and characterization of quaternary AlGaInN. A combination of photoluminescence (PL), high-resolution x-ray diffraction (XRD), and Rutherford backscattering spectrometry (RBS) characterizations enables us to explore the contours of constant- PL peak energy and lattice parameter as functions of the quaternary compositions. The observation of room temperature PL emission at 351nm (with 20% Al and 5% In) renders initial evidence that the quaternary could be used to provide confinement for GaInN (and possibly GaN). AlGaInN/GaInN MQW heterostructures have been grown; both XRD and PL measurements suggest the possibility of incorporating this quaternary into optoelectronic devices.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

Structural characterization of two K2SnX(PO4)3 (X=Fe,Yb) with langbeinite structure

2006 ◽  
Vol 21 (3) ◽  
pp. 214-219 ◽  
Author(s):  
Abderrahim Aatiq ◽  
Btissame Haggouch ◽  
Rachid Bakri ◽  
Youssef Lakhdar ◽  
Ismael Saadoune
Keyword(s):  
Solid State ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Cell Parameter ◽  
Rietveld Analysis ◽  
Conventional Solid State Reaction ◽  
X Ray ◽  
Octahedral Sites ◽  
Parameter Values

Structures of two K2SnX(PO4)3(X=Fe,Yb) phosphates, obtained by conventional solid state reaction techniques at 950 °C, were determined at room temperature by X-ray powder diffraction using Rietveld analysis. The two materials exhibit the langbeinite-type structure (P213 space group, Z=4). Cubic unit cell parameter values are: a=9.9217(4) Å and a=10.1583(4) Å for K2SnFe(PO4)3 and K2SnYb(PO4)3, respectively. Structural refinements show that the two crystallographically independent octahedral sites (of symmetry 3) have a mixed Sn∕X (X=Fe,Yb) population although ordering is stronger in the Yb phase than in the Fe phase.

scholarly journals Metal-Rich Metallaboranes: Synthesis, Structures and Bonding of Bi- and Trimetallic Open-Faced Cobaltaboranes

Inorganics ◽  
2021 ◽  
Vol 9 (4) ◽  
pp. 28
Author(s):  
Kriti Pathak ◽  
Chandan Nandi ◽  
Jean-François Halet ◽  
Sundargopal Ghosh
Keyword(s):  
Electronic Structures ◽  
Density Functional ◽  
Room Temperature ◽  
Electron Pair ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray ◽  
Cluster 2 ◽  
Cobalt Center

Synthesis, isolation, and structural characterization of unique metal rich diamagnetic cobaltaborane clusters are reported. They were obtained from reactions of monoborane as well as modified borohydride reagents with cobalt sources. For example, the reaction of [Cp*CoCl]2 with [LiBH4·THF] and subsequent photolysis with excess [BH3·THF] (THF = tetrahydrofuran) at room temperature afforded the 11-vertex tricobaltaborane nido-[(Cp*Co)3B8H10] (1, Cp* = η5-C5Me5). The reaction of Li[BH2S3] with the dicobaltaoctaborane(12) [(Cp*Co)2B6H10] yielded the 10-vertex nido-2,4-[(Cp*Co)2B8H12] cluster (2), extending the library of dicobaltadecaborane(14) analogues. Although cluster 1 adopts a classical 11-vertex-nido-geometry with one cobalt center and four boron atoms forming the open pentagonal face, it disobeys the Polyhedral Skeletal Electron Pair Theory (PSEPT). Compound 2 adopts a perfectly symmetrical 10-vertex-nido framework with a plane of symmetry bisecting the basal boron plane resulting in two {CoB3} units bridged at the base by two boron atoms and possesses the expected electron count. Both compounds were characterized in solution by multinuclear NMR and IR spectroscopies and by mass spectrometry. Single-crystal X-ray diffraction analyses confirmed the structures of the compounds. Additionally, density functional theory (DFT) calculations were performed in order to study and interpret the nature of bonding and electronic structures of these complexes.

Synthesis and Characterization of ZIF-8 Mixed Matrix Membranes

2014 ◽  
Vol 625 ◽  
pp. 661-664
Author(s):  
Chen Chuang Lok ◽  
Yin Fong Yeong
Keyword(s):  
Room Temperature ◽  
Synthesis Method ◽  
Mixed Matrix Membranes ◽  
Inorganic Filler ◽  
X Ray Diffraction ◽  
Mixed Matrix ◽  
Temperature Synthesis ◽  
X Ray ◽  
Matrix Membranes

In the present work, ZIF-8/6FDA-durene mixed matrix membranes (MMMs) were synthesized and characterized. ZIF-8 nanocrystals, which were used as the inorganic filler, were synthesized using rapid room-temperature synthesis method whereas 6FDA-durene polyimide was synthesized by polycondensation method followed by chemical imidization. Pure and 6FDA-durene membranes loaded with 5 wt%, 10 wt% and 15 wt% of ZIF-8 were fabricated. The structural properties and morphology of the resultant membranes were characterized by using X-ray Diffraction (XRD) and Field emission scanning electron microscope (FESEM) . The EDX images showed that ZIF-8 particles agglomerated in the polymer matrix. However, no phase separation was observed for all resultant MMMs.

Growth mechanism and characterization of ZnO nano-tubes synthesized using the hydrothermal-etching method

2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Yan Li ◽  
Chuan-Sheng Liu ◽  
Yun-Ling Zou
Keyword(s):  
Room Temperature ◽  
Morphological Analysis ◽  
Diffraction Field ◽  
X Ray Diffraction ◽  
X Ray ◽  
Room Temperature Photoluminescence ◽  
Etching Method ◽  
Nano Rods ◽  
Two Stages

AbstractZnO nano-tubes (ZNTs) have been successfully synthesized via a simple hydrothermal-etching method, and characterized by X-ray diffraction, field emission scanning electron microscopy and room temperature photoluminescence measurement. The as-synthesized ZNTs have a diameter of 500 nm, wall thickness of 20–30 nm, and length of 5 µm. Intensity of the plane (0002) diffraction peak, compared with that of plane (10$$ \bar 1 $$0) of ZNTs, is obviously lower than that of ZnO nano-rods. This phenomenon can be caused by the smaller cross section of plane (0002) of the nano-tubes compared with that of other morphologies. On basis of the morphological analysis, the formation process of nano-tubes can be proposed in two stages: hydrothermal growth and reaction etching process.

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