scholarly journals Synthesis of Novel Azo-Linked 5-Amino-Pyrazole-4-Carbonitrile Derivatives Using Tannic Acid–Functionalized Silica-Coated Fe3O4 Nanoparticles as a Novel, Green, and Magnetically Separable Catalyst

2021 ◽  
Vol 9 ◽  
Author(s):  
Farhad Sedighi Pashaki ◽  
Mohammad Nikpassand

Tannic acid–linked silica-coated Fe3O4 nanoparticles (Fe3O4@SiO2@Tannic acid) were prepared and characterized by transmission electron microscope (TEM), field emission scanning electron microscope (FE-SEM), X-ray powder diffraction (XRD), X-ray spectroscopy (EDX), vibrating sample magnetometry (VSM), and Fourier transform infrared (FT-IR) spectroscopy. Fe3O4@SiO2@Tannic acid supplies an environmentally friendly procedure for the synthesis of some novel 5-amino-pyrazole-4-carbonitriles through the three-component mechanochemical reactions of synthetized azo-linked aldehydes, malononitrile, and phenylhydrazine or p-tolylhydrazine. These compounds were produced in high yields and at short reaction times. The catalyst could be easily recovered and reused for six cycles with almost consistent activity. The structures of the synthesized 5-amino-pyrazole-4-carbonitrile compounds were confirmed by 1H NMR, 13C NMR, and FTIR spectra, and elemental analyses.

2020 ◽  
Vol 17 ◽  
Author(s):  
Mohammad Nikpassand ◽  
Zahra Pourkarim

Introduction: NiFe2O4@SiO2nPr@glucose catalyzed synthesis of novel 5-pyrazolin-1,2,4-triazazolidine-3- ones (thiones). Materials and Methods: Amino glucose‐ functionalized silica‐ coated NiFe2O4 nanoparticles (NiFe2O4@SiO2 nPr@glucose amine or NiFe2O4@SiP@GA) were synthesized and characterized by X-ray powder diffraction (XRD), X-ray spectroscopy (EDX), transmission electron microscope (TEM), field emission scanning electron microscope (FE-SEM), vibrating sample magnetometry (VSM) and fourier transform infrared spectroscopy (FT-IR). Results and Discussion: NiFe2O4@SiP@GA supply an eco-friendly procedure for the synthesis of some novel 5- pyrazolin-1,2,4-triazazolidine-3-ones or thiones through one-pot reaction of thiosemicarbazide (hydrazinecarbothioamide) and synthetized pyrazole carbaldehydes. These compounds were obtained in high yields in short reaction times. The catalyst could be easily recovered and reused for six cycles with almost consistent activity. The structures of the synthesized 5-pyrazolin-1,2,4-triazazolidine-3-ones or thiones were confirmed by 1H NMR, 13C NMR and FTIR spectral data and elemental analyses. Conclusion: In conclusion, we have investigated NiFe2O4@SiO2nPr@amino glucose as a new, eco-friendly, inexpensive, mild and reusable catalyst for the synthesis of 5-pyrazolin-1,2,4-triazazolidine-3-ones or thiones. High yield, a simple work‐ up procedure, adherence to the basics of green chemistry, environmental friendly and based on natural ingredients, ease of separation and recyclability of the magnetic catalyst and waste reduction are some advantages of this method.


2021 ◽  
Vol 3 (6) ◽  
Author(s):  
Kobra Nikoofar ◽  
Fatemeh Shahriyari

AbstractA simple, straightforward, and ultrasound-promoted method for the preparation of some highly functionalized tetrahydropyridines reported via pseudo five-component reaction of (hetero)aromatic aldehydes, different anilines, and alkyl acetoacetates in the presence of [N-CH2CO2H-3-pic]+HSO4−, as a novel ionic liquid, in green aqueous medium. The IL was synthesized utilizing simple and easily-handled substrates and characterized by FT-IR, 1H NMR, 13C NMR, GC-MASS, FESEM, EDX, and TGA/DTG techniques. The procedure contains some highlighted aspects which are: (a) performing the MCR in the presence of aqua and sonic waves, as two main important and environmentally benign indexes in green and economic chemistry, (b) high yields of products within short reaction times, (c) convenient work-up procedure, (d) preparing the new IL via simple substrates and procedure.


Author(s):  
Jeffrey A. Rood ◽  
Ashley L. Huttenstine ◽  
Zachery A. Schmidt ◽  
Michael R. White ◽  
Allen G. Oliver

Reaction of alkaline earth metal salts with diphenylphosphinic acid in dimethylformamide solvent afforded four coordination polymers: [Mg3(O2PPh2)6(DMF)2]·2DMF (I), [Ca(O2PPh2)2(DMF)2] (II), [Sr(O2PPh2)2(DMF)2] (III) and [Ba(O2PPh2)2(DMF)2] (IV) (where DMF isN,N-dimethylformamide). Single-crystal X-ray diffraction revealed that all four compounds produce linear chain structures in the solid state, with the Ca, Sr and Ba forming isostructural crystals. The bulk materials were characterized by FT–IR and1H NMR spectroscopy and elemental analyses.


2020 ◽  
Author(s):  
Arefeh Dehghani Tafti ◽  
Bi BiFatemeh Mirjalili ◽  
Abdolhamid Bamoniri ◽  
Naeimeh Salehi

Abstract Nano-egg shell/Ti(IV) (NEST) as a novel naturally based catalyst was prepared, characterized and applied for the synthesis of dihydropyrano[2,3-c]pyrazole [DHPP] derivatives. The characterization of NEST was performed using Fourier Transform Infrared (FT-IR) spectroscopy, X-ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), Energy-Dispersive X-ray Spectroscopy (EDX), and Thermo Gravimetric Analysis (TGA). DHPPs were synthesized in the presence of NEST via a four component reaction of aldehydes, ethyl acetoacetate, malononitrile and hydrazine hydrate at room temperature under solvent free conditions. The principal affairs of this procedure are easy work-up, high yields of pure products without the use of any toxic organic solvents, mild condition and short reaction times.


RSC Advances ◽  
2019 ◽  
Vol 9 (38) ◽  
pp. 22143-22152 ◽  
Author(s):  
Alexey Gusev ◽  
Elena Braga ◽  
Ekaterina Zamnius ◽  
Mikhail Kiskin ◽  
Mariya Kryukova ◽  
...  

A series of Zn(ii) complexes with 5-(4-R-phenyl)-3-(pyridin-2-yl)-1,2,4-triazoles have been synthesized and subsequently characterized by single crystal X-ray diffraction, 1H-NMR, FT-IR spectroscopy, elemental analyses, ESI-MS, and PXRD.


2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Kun Liu ◽  
Lianjie Zhu ◽  
Tengfei Jiang ◽  
Youguang Sun ◽  
Hongbin Li ◽  
...  

Mesoporous anatase TiO2micro-nanometer composite structure was synthesized by solvothermal method at 180°C, followed by calcination at 400°C for 2 h. The as-prepared TiO2was characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and Fourier transform infrared spectrum (FT-IR). The specific surface area and pore size distribution were obtained from N2adsorption-desorption isotherm, and the optoelectric property of the mesoporous TiO2was studied by UV-Vis absorption spectrum and surface photovoltage spectra (SPS). The photocatalytic activity was evaluated by photodegradation of sole rhodamine B (RhB) and sole phenol aqueous solutions under simulated sunlight irradiation and compared with that of Degussa P-25 (P25) under the same conditions. The photodegradation preference of this mesoporous TiO2was also investigated for an RhB-phenol mixed solution. The results show that the TiO2composite structure consists of microspheres (∼0.5–2 μm in diameter) and irregular aggregates (several hundred nanometers) with rough surfaces and the average primary particle size is 10.2 nm. The photodegradation activities of this mesoporous TiO2on both RhB and phenol solutions are higher than those of P25. Moreover, this as-prepared TiO2exhibits photodegradation preference on RhB in the RhB-phenol mixture solution.


2020 ◽  
Vol 43 (1) ◽  
pp. 117-124
Author(s):  
Javad Safaei-Ghomi ◽  
Zahra Samadi

AbstractFe3O4@SiO2-L-proline nanoparticles have been used as an effective catalyst for the preparation of pyrimidines by three-component reactions of 1,3-dimethylbarbituric acid, aromatic aldehydes and 4-methyl aniline or 4-methoxy aniline under reflux condition in ethanol. Fe3O4@SiO2-L-proline nanoparticles have been characterized by scanning electronic microscopy (SEM), powder X-ray diffraction (XRD), vibrating sample magnetometer (VSM), thermal gravimetric analysis (TGA), energy dispersive X-ray (EDS), dynamic light scattering (DLS) and FT-IR spectroscopy. This method provides several advantages including, the reusability of the catalyst, low catalyst loading, atom economy, short reaction times and high yields of products.


2014 ◽  
Vol 13 (03) ◽  
pp. 1450018 ◽  
Author(s):  
S. K. Kannan ◽  
M. Sundrarajan

In this study, the synthesis of a cerium oxide nanoparticle was carried out from Acalypha indica leaf extract. The synthesized nanoparticle was characterized by using X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive X-ray (EDX) and Transmission Electron Microscope (TEM) for structural confirmation. The studies clearly indicate that the synthesized CeO 2 nanoparticle is a crystalline material with particle size between 25–30 nm. Further analysis was carried out by Fourier Transform infrared spectroscopy (FT-IR), to provide evidence for the presence of Ce - O - Ce asymmetry stretching of the CeO 2 nanoparticle. Thermo Gravimetric and Differential Scanning Calorimetry analyses gave the thermal properties of cerium oxide nanoparticles. Antibacterial studies were conducted using the synthesized CeO 2. This result showed increasing rate of antibacterial behavior with gram positive and gram negative bacteria.


2021 ◽  
Vol 9 ◽  
Author(s):  
Leila Zare Fekri

Nanomagnetic dapsone-Cu supported on the silica-coated Fe3O4 (Fe3O4@SiO2-pr@dapsone-Cu) nanocomposite was synthesized and characterized by Fourier transform infrared (FT-IR), energy-dispersive X-ray (EDX), X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), zeta potential, vibrating sample magnetometer (VSM), and thermogravimetric analysis (TGA). This newly synthesized nanocomposite was chosen to act as a green, efficient, and recyclable Lewis acid for the multicomponent synthesis of new derivatives of pyrano[3,2-c]chromene-diones through the reaction of aromatic aldehydes, indandione, and 4-hydroxycoumarin in water. All of the synthesized compounds are new and are recognized by FT-IR, NMR, and elemental analysis; this avenue is new and has advantages such as short reaction times, high productivity, economical synthesis, and use of green solvent, H2O, as a medium. The catalyst is magnetically recoverable and can be used after six runs without a decrease in the efficiency.


2018 ◽  
Vol 36 (3) ◽  
pp. 419-426
Author(s):  
Nashiruddin Ahammed ◽  
Md Samim Hassan ◽  
Mehedi Hassan

AbstractIn this research article, pure and 1 %, 3 % and 5 % aluminium doped zinc oxide nanoparticles (NPs) were prepared via sol-gel method and then calcined at 500 °C. X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier transform infrared (FT-IR) spectroscopy, UV-Vis spectroscopy, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) techniques were used to investigate the structural, optical and thermal properties of synthesized pure and Al doped ZnO nanoparticles. Energy dispersive X-ray spectroscopy (EDX) analysis revealed high purity of nanoparticles in the synthesized products without any impurity peaks. Mean dimension of the nanoparticles was ~28 nm and they were hexagonal in shape, according to the images analyzed by transmission electron microscope (TEM). The optical absorption spectra of pure and Al doped ZnO samples studied using UV-Vis spectrometry have been presented and we have observed that the band gap increases with increasing Al concentration. In FT-IR spectra, the broad absorption peaks around 485 cm−1 and 670 cm−1 were assigned to Zn–O vibration. Above 450 °C, the TG curve became flat what means there was no weight loss. In the DSC curve it is seen that the transition at 150 °C was highly exothermic because of structural relaxation and on doping the exothermic peaks became shifted to the lower value of temperature. These types of materials are very useful in optoelectronics applications.


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