scholarly journals Green Synthesis of New Category of Pyrano[3,2-c]Chromene-Diones Catalyzed by Nanocomposite as Fe3O4@SiO2-Propyl Covalented Dapsone-Copper Complex

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.

Author(s):  
Masumeh Gilanizadeh ◽  
Behzad Zeynizadeh

A simple, green and highly efficient procedure has been developed for Knoevenagel condensation of malononitrile and aromatic aldehydes to the corresponding benzylidenemalononitriles in the presence of Fe3O4@APTMS@Zr-Sb-Ni-Zn nanoparticles (NPs) as a durable nanocatalyst. The heterogeneous nanocomposite was prepared by immobilization of Zr-Sb-Ni-Zn mixed metal oxides on APTMS-coated magnetite. The synthesized catalyst was characterized using Fourier-transform infrared spectroscopy (FT-IR), energy-dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), X-ray diffraction (XRD), vibration sample magnetometer (VSM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET). In this approach, the condensation of malononitrile and aromatic aldehydes were done in water under reflux conditions to give the corresponding products within 3-60 minutes in 89-95% yields. The magnetically recoverable catalyst was recycled and reused about four times without remarkable loss of activity. This method offers various benefits such as mild and eco-friendly reaction conditions, short reaction times and high purity of products, excellent efficiency and use of water as green solvent, reusability and recoverability of the nanostructure catalyst.


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.


2020 ◽  
Vol 8 ◽  
Author(s):  
Maryam Banazadeh ◽  
Sara Amirnejat ◽  
Shahrzad Javanshir

In this protocol, Fucoidan (FU), a fucose-rich sulfated polysaccharide extracted from brown algae Fucus vesiculosus was used for in situ preparation of magnetic Fe3O4@FU. Nanoco magnetic properties of Fe3O4@FU were investigated by energy dispersive X-ray (EDX) spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Brunauer–Emmett–Teller (BET) adsorption method, and vibrating sample magnetometer (VSM). The catalytic activity of Fe3O4@FU was employed for the synthesis of tri- and tetra-substituted imidazoles through three- and four-component reactions respectively, between benzyl, aldehydes, NH4OAc and benzyl, aldehydes, NH4OAc, and amine under reflux in ethanol. It is worth nothing that excellent yields, short reaction times, chromatography-free purification, and environmental friendliness are highlighted features of this protocol.


Crystals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 456
Author(s):  
Fahad A. Alharthi ◽  
Hamdah S. Alanazi ◽  
Amjad Abdullah Alsyahi ◽  
Naushad Ahmad

This study demonstrated the hydrothermal synthesis of bimetallic nickel-cobalt tungstate nanostructures, Ni-CoWO4 (NCW-NPs), and their phase structure, morphology, porosity, and optical properties were examined using X-ray Diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscopy- energy dispersive X-ray spectroscopy (SEM-EDS), high resolution Transmission electron microscopy (HR-TEM), Brunauer-Emmett-Teller (BET) and Raman instruments. It was found that as-calcined NCW-NPs have a monoclinic phase with crystal size ~50–60 nm and is mesoporous. It possessed smooth, spherical, and cubic shape microstructures with defined fringe distance (~0.342 nm). The photocatalytic degradation of methylene blue (MB) and rose bengal (RB) dye in the presence of NCW-NPs was evaluated, and about 49.85% of MB in 150 min and 92.28% of RB in 90 min degraded under visible light. In addition, based on the scavenger’s study, the mechanism for photocatalytic reactions is proposed.


2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  

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.


2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.


Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1725 ◽  
Author(s):  
Xiaohong Liu ◽  
Ming Li ◽  
Xuemei Zheng ◽  
Elias Retulainen ◽  
Shiyu Fu

As a type of functional group, azo-derivatives are commonly used to synthesize responsive materials. Cellulose nanocrystals (CNCs), prepared by acid hydrolysis of cotton, were dewatered and reacted with 2-bromoisobuturyl bromide to form a macro-initiator, which grafted 6-[4-(4-methoxyphenyl-azo) phenoxy] hexyl methacrylate (MMAZO) via atom transfer radical polymerization. The successful grafting was supported by Fourier transform infrared spectroscopy (FT-IR) and Solid magnetic resonance carbon spectrum (MAS 13C-NMR). The morphology and surface composition of the poly{6-[4-(4-methoxyphenylazo) phenoxy] hexyl methacrylate} (PMMAZO)-grafted CNCs were confirmed with Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The grafting rate on the macro-initiator of CNCs was over 870%, and the polydispersities of branched polymers were narrow. The crystal structure of CNCs did not change after grafting, as determined by X-ray diffraction (XRD). The polymer PMMAZO improved the thermal stability of cellulose nanocrystals, as shown by thermogravimetry analysis (TGA). Then the PMMAZO-grafted CNCs were mixed with polyurethane and casted to form a composite film. The film showed a significant light and pH response, which may be suitable for visual acid-alkali measurement and reversible optical storage.


2015 ◽  
Vol 68 (8) ◽  
pp. 1293 ◽  
Author(s):  
Pakvipar Chaopanich ◽  
Punnama Siriphannon

Hydroxyapatite (HAp) nanoparticles were successfully synthesized from an aqueous mixture of Ca(NO3)2·4H2O and (NH4)2HPO4 by a facile single-step refluxing method using polystyrene sulfonate (PSS) as a template. The effects of reaction times, pH, and PSS concentration on the HAp formation were investigated. It was found that the crystalline HAp was obtained under all conditions after refluxing the precursors for 3 and 6 h. The longer refluxing time, the greater the crystallinity and the larger the crystallite size of the HAp nanoparticles. The HAp with poor crystallinity was obtained at pH 8.5; however, the well-crystallized HAp was obtained when reaction pH was increased to 9.5 and 10.5. In addition, the X-ray diffraction patterns revealed that the presence of PSS template caused the reduction of HAp crystallite size along the (002) plane from 52.6 nm of non-template HAp to 43.4 nm and 41.4 nm of HAp with 0.05 and 0.2 wt-% PSS template, respectively. Transmission electron microscopy images of the synthesized HAp revealed the rod-shaped crystals of all samples. The synthesized HAp nanoparticles were modified by l-aspartic acid (Asp) and l-arginine (Arg), having negative and positive charges, respectively. It was found that the zeta potential of HAp was significantly changed from +5.46 to –24.70 mV after modification with Asp, whereas it was +4.72 mV in the Arg-modified HAp. These results suggested that the negatively charged amino acid was preferentially adsorbed onto the synthesized HAp surface.


2021 ◽  
Vol 11 (3) ◽  
pp. 215
Author(s):  
Achraf El Hallaoui ◽  
Tourya Ghailane ◽  
Soukaina Chehab ◽  
Youssef Merroun ◽  
Rachida Ghailane ◽  
...  

<p>This work aims to prepare a new bimetallic phosphate catalyst using a new simple and effective method. This new catalyst was ready for the first time by a modification of Triple Super Phosphate (TSP) fertilizer with silver sulfate (AgSO<sub>4</sub>), followed by the impregnation of the aluminum atoms using aluminum nitrate (Al(NO<sub>3</sub>)<sub>3</sub>). The use of Al/Ag<sub>3</sub>PO<sub>4</sub>, for the first time as a heterogeneous catalyst in organic chemistry, offers a new, efficient, and green pathway for synthesizing 1,2-dihydro-l-phenyl-3H-naphth[1,2-e]-[1,3]oxazin-3-one derivatives by one-pot three-component cyclocondensation of b-naphthol, aryl aldehyde, and urea. The structure and the morphology of the prepared catalyst were characterized by spectroscopic methods such as X-Ray Diffraction (XRD), Fourier Transform Infrared spectroscopy (FT-IR), and dispersive X-ray spectrometry coupled with a scanning electron microscope (EDX-SEM). In addition, the optimization of the reaction parameters was carried out considering the effect of catalyst amount, the temperature, and the solvent. The procedure described herein allowed a comfortable preparation of oxazine derivatives with excellent yields, short reaction times, and in the absence of organic solvent.</p>


2021 ◽  
Vol 66 ◽  
pp. 61-71
Author(s):  
Tahereh Heidarzadeh ◽  
Navabeh Nami ◽  
Daryoush Zareyee

The principal aim of this research is using biosynthesized ZnO-CaO nanoparticles (NPs) for preparation of indole derivatives. ZnO-CaO NPs have been prepared using Zn(CH3COO)2 and eggshell waste powder in solvent-free conditions. Morphology and structure of NPs were determined by FT-IR, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy dispersive spectra (EDS). It was used as a highly efficient catalyst for the synthesis of indole derivatives. Some indole derivatives were synthesized by the reaction of indole, formaldehyde, aromatic and aliphatic amines in the presence of ZnO-CaO NPs (5 mol%) in ethanol under reflux conditions. The assigned structure was further established by CHN analyses, NMR, and FT-IR spectra. Because of excellent capacity, the exceedingly simple workup and good yield, eco-friendly catalyst ZnO-CaO NPs were proved to be a good catalyst for this reaction.


Sign in / Sign up

Export Citation Format

Share Document