Microwave-assisted solvent-free synthesis and spectral and structural characterization of cyclotriphosphazene hexakis(o-tolylamide)

2018 ◽  
Vol 73 (12) ◽  
pp. 999-1003 ◽  
Author(s):  
Mohammad Hakimi ◽  
Homeyra Rezaei ◽  
Keyvan Moeini ◽  
Heidar Raissi ◽  
Vaclav Eigner ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Microwave Irradiation ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
Microwave Assisted ◽  
Ft Ir ◽  
Solvent Free Synthesis

AbstractA new cyclotriphosphazene, 2,2,4,4,6,6-hexakis (o-tolylamono)-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinine (MPAP), was prepared using microwave irradiation and identified by elemental analysis, FT-IR, Raman, 31P NMR spectroscopy, and single-crystal X-ray diffraction. In the crystal, in addition to hydrogen bonds, the network is further stabilized by inter- and intramolecular π–π stacking interactions between aromatic rings.

Synthesis and Characterization of Three Novel Nitrogen-containing Macrolides

2011 ◽  
Vol 66 (9) ◽  
pp. 930-934
Author(s):  
Xin Leng ◽  
Bingqin Yang ◽  
Yuanyuan Liu ◽  
Yi Xie ◽  
Jie Tong
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
1H Nmr Spectroscopy ◽  
Mass Spectra ◽  
Synthesis And Characterization ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Preparation Methods ◽  
X Ray

Three novel nitrogen-containing macrolides have been synthesized by esterification. All of them have been characterized by infrared (IR), elemental analysis, mass spectra (MS), and 1H NMR spectroscopy, and their crystal structures were determined by single-crystal X-ray diffraction. The preparation methods and the intermolecular associations based on C-H・・・O hydrogen bonds and π- π stacking interactions are discussed.

One Step Synthesis and Characterization of Zirconia-Graphene Composites

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  
Keyword(s):  
Synthesis And Characterization ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Graphene Composite ◽  
Transmission Electron ◽  
One Step ◽  
Ft Ir ◽  
Xrd Techniques

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.

Nitroxide radicals appended to phthalonitriles: synthesis, structural characterization and photophysical properties

2021 ◽  
Vol 77 (3) ◽  
pp. 137-143
Author(s):  
Ismail Fidan ◽  
Emel Onal ◽  
Catherine Hirel
Keyword(s):  
Magnetic Measurements ◽  
Photophysical Properties ◽  
Nucleophilic Aromatic Substitution ◽  
Structural Studies ◽  
Aromatic Substitution ◽  
Nitronyl Nitroxide ◽  
X Ray Diffraction ◽  
X Ray ◽  
Microwave Assisted ◽  
Ft Ir

The syntheses of 4-[4-(4,4,5,5-tetramethyl-2-imidazoline-3-oxide-1-oxyl-2-yl)phenoxy]phthalonitrile (3, C21H19N4O3) and 4-[4-(4,4,5,5-tetramethyl-2-imidazoline-1-oxyl-2-yl)phenoxy]phthalonitrile (4) were carried out by microwave-assisted nucleophilic aromatic substitution of 4-nitrophthalonitrile (2) by the pre-formed 2-(4-hydroxyphenyl)-4,4,5,5-tetramethyl-2-imidazoline-3-oxide-1-oxyl (1). Compounds 3 and 4 were characterized unambiguously by a rich array of analyses, such as melting point, FT–IR, MALDI–TOF MS, elemental analysis, UV–Vis, CV, EPR, magnetic measurements and single-crystal X-ray diffraction. Structural studies demonstrate that the C—H...X and C—X...π (X = O and N) interactions in the radical nitronyl nitroxide groups play an important role in the assembly of the crystal structures. Moreover, cyclic voltammetry analyses show that the phthalonitrile substituent retains the redox properties of the Ullman radicals.

Rapid Synthesis and Characterization of CuInS2 Prepared Using Microwave-Assisted Heating

2015 ◽  
Vol 775 ◽  
pp. 143-146
Author(s):  
Ming Kwen Tsai ◽  
Yueh Chien Lee ◽  
Chia Chih Huang ◽  
Sheng Yao Hu ◽  
Kwong Kau Tiong ◽  
...  
Keyword(s):  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Structural And Optical Properties ◽  
Rapid Synthesis ◽  
X Ray ◽  
Sem Image ◽  
Microwave Assisted ◽  
Calcination Treatment ◽  
Scanning Electron

In this work, the CuInS2 nanoparticles are successfully synthesized by microwave-assisted heating technique and further calcined at 400 °C. The morphological, structural, and optical properties of the synthesized CuInS2 nanoparticles are investigated by scanning electron microscope (SEM), X-ray diffraction (XRD), Raman scattering, and transmittance measurement, respectively. The SEM image shows the clear particle shape of the calcined CuInS2 nanoparticles. After calcination treatment, the fundamental (112) peak of the XRD spectrum and a broad Raman peak mixed with chalcopyrite and CuAu structures support the improved crystallinity of the calcined CuInS2 nanoparticles.

Structural, spectral and docking studies of a coordination polymer of zinc(II) formed by a pyridine-derived linker

2018 ◽  
Vol 73 (6) ◽  
pp. 369-375 ◽  
Author(s):  
Farzin Marandi ◽  
Keyvan Moeini ◽  
Fereshteh Alizadeh ◽  
Zahra Mardani ◽  
Ching Kheng Quah ◽  
...  
Keyword(s):  
Coordination Polymer ◽  
Docking Studies ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Docking Calculations ◽  
Ft Ir ◽  
Zinc Coordination ◽  
Linear Coordination

AbstractA mixed ligand zinc coordination polymer, {Zn(μ-DPE)(DBM)2}n (1) (HDBM: dibenzoylmethane and DPE: (E)-1,2-di(pyridin-4-yl)ethene), was prepared and identified by elemental analysis, FT-IR, 1H NMR spectroscopy and single-crystal X-ray diffraction. In the 1D linear coordination polymer of 1, the zinc atom has a ZnN2O4 environment with octahedral geometry. These complex units are linked by the bridging of the planar N2 donor DPE ligands. In the coordination network of complex 1, in addition to the hydrogen bonds, the network is more stabilized by π–π stacking interactions between pyridine and β-diketone moieties of the ligands. These interactions increase the ability of the compound to interact with biomacromolecules (BRAF kinase, CatB, DNA gyrase, HDAC7, rHA, RNR, TrxR, TS and Top II) as investigated by docking calculations.

The Characterization of Bovine Bone-Derived Hydroxyapatite Isolated Using Novel Non-Hazardous Method

2020 ◽  
Vol 45 ◽  
pp. 49-56
Author(s):  
Aniek Setiya Budiatin ◽  
Samirah ◽  
Maria Apriliani Gani ◽  
Wenny Putri Nilamsari ◽  
Chrismawan Ardianto ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Extraction Method ◽  
Bovine Bone ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
Novel Method ◽  
Scanning Electron

Bovine bone is a considerable source for the production of hydroxyapatite. The recent study reported a novel method to extract hydroxyapatite from bovine bone without producing hazardous residue. The bovine bones were cut and boiled in the opened chamber followed by boiling in pressurized tank. The bones were then soaked into 95% ethanol. Calcination was then conducted in 800°C, 900°C and 1,000°C, for 2 hours. The result was then grinded and sieved. The powder then was characterized using Fourier transform infrared (FT-IR), Scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD) to measure the purity of hydroxyapatite. It is concluded that the hydroxyapatite derived from this process showed 100% purity, resulting 35.34 ± 0.39% w/w from the wet bone weight and 72.3% w/w from the dried weight. The present extraction method has been proven to yield high amount of pure hydroxyapatite as well as reducing the use of hazardous reagent.

scholarly journals Synthesis, Crystal Structures, and Spectroscopic Characterization of Bis-aldehyde Monomers and Their Electrically Conductive Pristine Polyazomethines

Polymers ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 1498 ◽  
Author(s):  
Abdul Hafeez ◽  
Zareen Akhter ◽  
John F. Gallagher ◽  
Nawazish Ali Khan ◽  
Asghari Gul ◽  
...  
Keyword(s):  
Electrical Conductivity ◽  
Spectroscopic Characterization ◽  
Spectroscopic Techniques ◽  
Conductivity Measurements ◽  
X Ray Diffraction ◽  
Electrically Conductive ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Ft Ir

Bis-aldehyde monomers 4-(4′-formyl-phenoxy)benzaldehyde (3a), 3-methoxy-4-(4′-formyl-phenoxy)benzaldehyde (3b), and 3-ethoxy-4-(4′-formyl-phenoxy)benzaldehyde (3c) were synthesized by etherification of 4-fluorobenzaldehyde (1) with 4-hydroxybenzaldehyde (2a), 3-methoxy-4-hydroxybenzaldehyde (2b), and 3-ethoxy-4-hydroxybenzaldehyde (2c), respectively. Each monomer was polymerized with p-phenylenediamine and 4,4′-diaminodiphenyl ether to yield six poly(azomethine)s. Single crystal X-ray diffraction structures of 3b and 3c were determined. The structural characterization of the monomers and poly(azomethine)s was performed by FT-IR and NMR spectroscopic techniques and elemental analysis. Physicochemical properties of polymers were investigated by powder X-ray diffraction, thermogravimetric analysis (TGA), viscometry, UV–vis, spectroscopy and photoluminescence. These polymers were subjected to electrical conductivity measurements by the four-probe method, and their conductivities were found to be in the range 4.0 × 10−5 to 6.4 × 10−5 Scm−1, which was significantly higher than the values reported so far.

Imidazole-containing Bispidine Ligands: Synthesis, Structure and Cu(II) Complexation

2011 ◽  
Vol 66 (7) ◽  
pp. 721-728 ◽  
Author(s):  
Martin Walther ◽  
Madlen Matterna ◽  
Stefanie Juran ◽  
Silke Fähnemann ◽  
Holger Stephan ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Enol Form ◽  
Trans Configuration ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Impact ◽  
Configurational Isomerism

The preparation and characterization of tris-pyridyl bispidine (3,7-diazabicyclo[3.3.1]nonane) derivatives with benzimidazole and imidazole donor groups at the N-3 position of the bispidine skeleton and their copper(II) complexes are reported. The impact of the hetaryl substituents on the configurational isomerism of piperidones and their corresponding bispidones has been studied by NMR spectroscopy, revealing the exclusive appearance in the enol form for the piperidones in solution and the trans-configuration regarding the two pyridyl substituents, as well as the sole formation of the unsymmetric exo-endo isomers for the corresponding bispidones. Thus, the bispidones are preorganized ligands for building pentacoordinated complexes, confirmed by the preparation and characterization of the corresponding Cu(II) complexes. Of the di-pyridyl piperidones with benzimidazole and imidazole substituents, and of the Cu(II) complex of the benzimidazole-containing bispidone, crystals have become available for the analysis by X-ray diffraction, showing that the piperidones form the enol tautomers also in the solid state.

Characterization of Electrospun Poly(Lactic Acid)/polyaniline Blend Nanofibers

2011 ◽  
Vol 332-334 ◽  
pp. 317-320 ◽  
Author(s):  
Hui Qin Zhang
Keyword(s):  
Lactic Acid ◽  
Composite Nanofibers ◽  
Weight Ratio ◽  
Electrospinning Process ◽  
Poly Lactic Acid ◽  
X Ray Diffraction ◽  
Sem Images ◽  
X Ray ◽  
Ft Ir

In this study, composite nanofibers of polyaniline doped with dodecylbenzene sulfonic acid (PANI-DBSA) and Poly(lactic acid) (PLA) were prepared via an electrospinning process. The surface morphology, thermal properties and crystal structure of PLA/PANI-DBSA nanofibers are characterized using Fourier transform infrared spectroscopy (FT-IR), wide-angle x-ray diffraction (WAXD) and scanning electron microscopy (SEM). SEM images showed that the morphology and diameter of the nanofibers were affected by the weight ratio of blend solution.

Preparation and Electrical Characterization of Poly(Aniline) NanoClay Composites

2015 ◽  
Vol 34 (4) ◽  
Author(s):  
Esma Ahlatcioǧlu ◽  
Bahire Filiz şenkal ◽  
Mustafa Okutan
Keyword(s):  
Electrical Characterization ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Ft Ir ◽  
Doped Polyaniline ◽  
Poly Aniline ◽  
Scanning Electron

AbstractIn this work, synthesis and characterization of composite materials based on NanoClay(NC) and boric acid doped PolyAniline (PANI) is studied. PANI was successfully incorporated into NC to form PANI-NC composites. The resulting organic-inorganic hybrid material, PANI-NC was characterized by various physicochemical techniques. Formation of PANI inside the clay tactoid has been confirmed by X-ray diffraction studies (XRD), scanning electron microscope (SEM) and FT-IR. Also, conductivity and physical properties of the PANI-NC composites were investigated.

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