scholarly journals One Pot Ultrasonic Assisted {[Ni(tptz)Cl(H2O)2][Ni(tptz)(H2O)3]}-3Cl.5H2O Complex Formation Using Triazine Ligand, XRD/HSA-Interactions, and Spectral and Thermal Investigation

Crystals ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1474
Author(s):  
Abeer A. AlObaid ◽  
Ahmed Boshaala ◽  
Younis O. Ben Amer ◽  
Abrahem F. Abrahem ◽  
Nabil Al-Zaqri ◽  
...  

Under room temperature ultrasonic conditions, mixing the neutral 2,4,6-tri(pyridin-2-yl)-1,3,5-triazine (tptz) ligand with Ni(II) salt resulted in the preparation of a unique {[Ni(tptz)Cl(H2O)2]-[Ni(tptz)(H2O)3]}3Cl.5H2O complex with two different nickel(II) centers in a high yield. The crystal structure of {[Ni(tptz)Cl(H2O)2][Ni(tptz)(H2O)3]}3Cl.5H2O revealed the existence of distorted octahedral around both Ni(II) centers. The complex structure was further supported by FT-IR, UV-Vis., CHN-EA, TGA and EDX. The computed HSA was also performed to support the XRD interaction types. The existence of the H2O molecules in the crystal lattice was examined by FT-IR and TG/DTG measurements that proved the presence of coordinated and uncoordinated water molecules. Moreover, the thermal stability of the desired complex was evaluated at open atmosphere via TG/DTG and showed stability up to ~400 °C and multistep thermal decomposition.

SynOpen ◽  
2021 ◽  
Author(s):  
Mina Ghassemi ◽  
Ali Maleki

Copper ferrite (CuFe2O4) magnetic nanoparticles (MNPs) were synthesized via thermal decomposition method and applied as a reusable and green catalyst in the synthesis of functionalized 4H-pyran derivatives using malononitrile, an aromatic aldehyde and a β-ketoester in ethanol at room temperature. Then it was characterized by Fourier transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy (EDX) analysis, scanning electron microscopy (SEM) images, thermo gravimetric and differential thermo gravimetric (TGA/DTG) analysis. The catalyst was recovered from the reaction mixture by applying an external magnet and decanting the mixture. Recycled catalyst was reused for several times without significant loss in its activity. Running the one-pot three-component reaction at room temperature, no use of eternal energy source and using a green solvent provide benign, mild, and environmentally friendly reaction conditions; as well, ease of catalyst recovering, catalyst recyclability, no use of column chromatography and good to excellent yields are extra advantages of this work.


2018 ◽  
Vol 9 (1) ◽  
pp. 39-49 ◽  
Author(s):  
Sharifah Nurul Ain Syed Hashim ◽  
Sarani Zakaria ◽  
Chin Hua Chia ◽  
Sharifah Nabihah Syed Jaafar

In this study, soda alkali lignin from oil palm empty fruit bunch (EFB-AL) and kenaf core (KC-AL) are esterified with maleic anhydride under two different conditions, namely i) pyridine at temperature of 120°C for 3h and ii) aqueous alkaline solution at room temperature for 4h. As a result, the weight percentage gain (WPG) of the esterified EFB-AL (EFB-EL) and esterified KC-AL (KC-EL) in pyridine demonstrated a higher compared to aqueous alkaline solution. The FT-IR results of EFB-EL and KC-EL in both solvents exhibited some changes at the carbonyl and hydroxyl groups. Furthermore, the esterification process induced the carboxylic peak to appear in both alkali lignin samples. The outcome is confirmed by conducting H-NMR analysis, which demonstrated ester and carboxylic acid peaks within the spectral analysis. Finally, the TGA results showed both EFB-EL and KC-EL that are exposed to aqueous alkaline actually possessed better thermal stability and higher activation energy (Ea) compared to the esterified samples in pyridine.


2016 ◽  
Vol 5 (4) ◽  
Author(s):  
Ramadan Ahmed Mekheimer ◽  
Abdullah Mohamed Asiri ◽  
Afaf Mohamed Abdel Hameed ◽  
Reham R. Awed ◽  
Kamal Usef Sadek

AbstractStarting from readily available 2-naphthol, aldehydes, aryl and alkylamines, a variety of Betti bases were efficiently synthesized utilizing a catalytic amount of cerium (IV) ammonium nitrate (CAN) at room temperature. This protocol has advantages of high yield, mild reaction conditions, no environmental pollution, diversity of reactants and simple work up procedure.


2012 ◽  
Vol 68 (8) ◽  
pp. m209-m212 ◽  
Author(s):  
Jiang-Hong Fu ◽  
Yu-Ling Wang ◽  
Ying Chen ◽  
Chang-Hui Hu ◽  
Li Tang

The title compound, [CuNa(C4H3O7S)(C10H8N2)(H2O)3]n, consists of one CuIIcation, one NaIcation, one 2-sulfonatobutanedioate trianion (SSC3−), one 2,2′-bipyridyl (bpy) ligand and three coordinated water molecules as the building unit. The coordination of the CuIIcation is composed of two pyridyl N atoms, one water O atom and two carboxylate O atoms in a distorted square-pyramidal coordination geometry with an axial elongation. The NaIcation is six-coordinated by three water molecules and three carboxylate O atoms from three SSC3−ligands in a distorted octahedral geometry. Two SSC3−ligands link two CuIIcations to form a Cu2(SSC)2(bpy)2macrocyclic unit lying across an inversion centre, which is further linked by NaIcationsviaNa—O bonds to give a one-dimensional chain. Interchain hydrogen bonds link these chains to form a two-dimensional layer, which is further extended into a three-dimensional supramolecular framework through π–π stacking interactions. The thermal stability of the title compound has also been investigated.


Author(s):  
D. V. Golubev ◽  
V. D. Rumyantseva ◽  
V. V. Fomichev

For the first time, a complex of bismuth(III) with iodine and etioporphyrin II is reported. It was prepared by reacting etioporphyrin II and bismuth(III) iodide in pyridine in Ar atmosphere. The prepared compound was characterized by FT-IR, 1H-NMR, UV-VIS spectroscopy and mass spectrometry. One intense line at m/z 684.990 attributed to the complex without the iodine atom is observed in the mass spectrum. This is in agreement with the data indicating that bismuthporphyrin complexes generally have low stability. Analysis of FT-IR spectra obtained at room temperature and at 145°С is reported. Priroda15 DFT package was used for optimization of complex geometry and calculation of the IR spectrum. Calculations were done using BPE functional and L1 basis set under relativistic approximation of Dyall Modified Dirac. Assignment of the vibrational frequencies is reported. Collected data indicate that the complex of bismuth(III) with iodine and etioporphyrin II is not stable and easily hydrolyses when exposed to air forming the corresponding hydroxocomplex. This transformation does not change significantly the dynamics of the porphyrin ring.


Author(s):  
Jie Ma ◽  
Wen-Zhi Zhang ◽  
Jie Xiong ◽  
Chun-Yan Yan

The title coordination polymer, {[Co2(C12H7NO8)(H2O)6]·5H2O} n , was crystallized at room temperature from an aqueous solution of 2-aminodiacetic terephthalic acid (H4adtp) and cobalt(II) nitrate. The asymmetric unit consists of one adtp4− ligand, one and two half CoII ions, six water ligands coordinated to CoII ions and five uncoordinated water molecules. Two of the cobalt cations lie on centres of inversion and are coordinated in octahedral O2(OH2)4 environments, whereas the other adopts a slightly distorted octahedral NO3(OH2)2 environment. The crystal structure contains parallel stacked, one-dimensional zigzag chains, {[Co2(C12H7NO8)(H2O)6]} n , which assemble into a three-dimensional supramolecular architecture via networks of hydrogen bonds involving the coordinated and free water molecules. One-dimensional `water tapes' are formed, containing alternating six-membered and twelve-membered rings of water molecules, together with water pentamers, in which a central uncoordinated water molecule is hydrogen bonded to two coordinated and two free water molecules in a tetrahedral arrangement.


2021 ◽  
Vol 8 ◽  
Author(s):  
Fa-Jie Chen ◽  
Zhenguo Hua ◽  
Jianhui Chen ◽  
Jiajia Chen ◽  
Daesung Lee ◽  
...  

Herein, we report an efficient method for the synthesis of (Z)-β-halovinyl ketones through a one-pot Sonogashira coupling and hydrohalogenation reaction promoted by palladium-copper catalyst and Brønsted acid. The ynone intermediates are generated in situ from readily available acid chlorides and terminal alkynes at room temperature, which are directly converted to (Z)-β-halovinyl ketones by treating with triflic acid. This method avoids the use of an external halogen source and features broad substrate scope, high yield, and good to excellent stereoselectivity.


Catalysts ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 1000
Author(s):  
Iqbal ◽  
Sadiq ◽  
Sadiq ◽  
Ullah ◽  
Fazal ◽  
...  

A simple and practical procedure has been adopted for one pot synthesis of benzimidazole derivatives under mild reaction conditions, starting from cinnamyl alcohol (COH) with bimetallic nanoparticles (BNPs) and supported bimetallic nanoparticles of Cu, Ti, Zn, Mn, Ag, and Co. All the catalysts were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), X-Ray Diffractometry (XRD), Brunauer Emmett-Teller (BET) surface area, and pore size analyzer. The products were identified/quantified with 1HNMR, FT-IR, and MS. 98% yield of substituted derivatives of benzimidazole was obtained with Cu–Ti supported on FMWCNTs in ethanol with excellent selectivity. Quantum chemical calculations of molecular reactivity of substituted cinnamaldehyde (CHO) and ortho phenylenediamine (OPD) have good consistency with experimental results. The returns of this work were the use of readily available catalysts, high yield, short reaction time, and simplicity of the process.


2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Thupakula Venkata Madhukar Sreekanth ◽  
Patnamsetty Chidanandha Nagajyothi ◽  
Gutturu Rajasekhara Reddy ◽  
Jaesool Shim ◽  
Kisoo Yoo

Abstract This study describes a simple, high-yield, rapid, and inexpensive route for the synthesis of cubic shape-like cerium oxide nanocubes (CeO2 NCs) using different urea concentrations (0.5, 1.0, and 2.0 g) by the hydrothermal method. The synthesized nanocubes (NCs) are labeled as CeO2 NCs-0.5, CeO2 NCs-1.0, and CeO2 NCs-2.0, corresponding to 0.5, 1.0, and 2.0 g of urea, respectively. The synthesized NCs were characterized by FT-IR, UV-visible, XRD, XPS, SEM and HR-TEM analysis. The synthesized NCs were cubic in shape with average sizes of 12, 12, and 13 nm for the CeO2 NCs-0.5, CeO2 NCs-1.0, and CeO2 NCs-2.0, respectively, obtained by the XRD analysis. The catalytic activity of the CeO2 NCs was studied for the purpose of obtaining the reduction of malachite green (MG) in the presence of sodium borohydride (NaBH4) at room temperature.


2016 ◽  
Vol 30 (11) ◽  
pp. 1650227 ◽  
Author(s):  
A. R. Bahador ◽  
M. Molaei ◽  
M. Karimipour

In this work, a one-pot, rapid, green and room temperature photochemical synthesis of transition metal (TM; Cu, Mn)-doped ZnSe nanocrystals (NCs) was reported. NCs were successfully characterized using Fourier transform-infrared (FT-IR), photoluminescence (PL) and UV-Visible (UV-Vis) spectroscopy, transmission electron microscopy (TEM), X-ray diffractometry (XRD) and energy dispersive X-ray spectra (EDX). FT-IR spectra confirmed the capping of ZnSe by thioglycolic acid (TGA) molecules. XRD and TEM analysis demonstrated zinc blend phase NCs with an average size of around 3 nm. Band gap of ZnSe NCs was about 3.6 eV which it was decreased by increasing the illumination time. PL spectra of ZnSe NCs showed a broad emission with two peaks located at 380 nm and 490 nm related to excitonic and trap states emission, respectively. For ZnSe:Cu NCs, excitonic emission disappeared completely and PL intensity of trap states emission increased with the increase in the Cu[Formula: see text] ion concentration so that for precursor ratio of Cu:Zn 1%, optimal value of PL intensity was obtained. For ZnSe:Mn NCs, the excitonic emission decreased gradually with the increase in the impurity concentration whereas trap state emission increased. Moreover, a peak about 590 nm was appeared from 4T1-6A1 transition of the Mn[Formula: see text] impurity, demonstrating the Mn incorporation inside the ZnSe NCs structure.


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