Facile synthesis of pyrazole derivatives using reusable Fe3O4@MCM-41-SO3H

2021 ◽  
pp. 1-8
Author(s):  
Samanehsadat Sharifi ◽  
Malek Taher Maghsoudlou ◽  
Nourallah Hazeri

In this research, Fe3O4-MCM-41-SO3H was synthesized as a magnetically reusable Lewis acid catalyst and used in the cyclization reaction of 3-acylcoumarins or 3-chromonecarboxylic acid with arylhydrazine derivatives for the synthesis of pyrazoles in high yields under solvent-free conditions and with a simple work-up process. Fe3O4-MCM-41-SO3H was characterized by Fourier transform infrared (FTIR), scanning electron microscopy (SEM), and X‐ray diffraction (XRD) analyses.

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Arefeh Dehghani Tafti ◽  
Bi Bi Fatemeh Mirjalili ◽  
Abdolhamid Bamoniri ◽  
Naeimeh Salehi

AbstractNano-eggshell/Ti(IV) as a novel naturally based catalyst was prepared, characterized and applied for the synthesis of dihydropyrano[2,3-c]pyrazole derivatives. The characterization of nano-eggshell/Ti(IV) was performed using Fourier Transform Infrared spectroscopy, X-ray Diffraction, Field Emission Scanning Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and Thermo Gravimetric Analysis. Dihydropyrano[2,3-c]pyrazoles were synthesized in the presence of nano-eggshell/Ti(IV) 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 mild condition, short reaction times, easy work-up, high yields, reusability of the catalyst and the absence of toxic organic solvents.


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.


2012 ◽  
Vol 442 ◽  
pp. 3-7
Author(s):  
Qian Ming Wang ◽  
Zheng Yang Zhang ◽  
Yan Li

Cerium and gadolinium phosphate micro-meter size phosphors with average diameters of 20-50 μM were prepared. X-Ray Diffraction (XRD) data confirmed the crystalline phases of samples could be formed at different temperature. Scanning electron microscopy (SEM) investigated the morphology and crystalline of the samples, showing that many regular and large pores (100-200 μM) were dispersed within the micro-meter scale composites. We have proved the above crystal growth structures were controllable and predicable based on the current conditions.


2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Pullar Vadivel ◽  
Rathinam Ramesh ◽  
Appaswami Lalitha

An effective one-pot three-component reaction of aromatic aldehydes with 1,3-diketone and urea or thiourea under solvent-free condition leads to the formation of mono- and bis-dihydropyrimidin-2-(1H)-ones using Ce-MCM-41 as a recyclable solid acid catalyst. This method has several advantages like simple and easy work-up with shorter reaction time, reusability of catalyst, and high yields of Biginelli products.


2018 ◽  
Vol 11 (06) ◽  
pp. 1840003 ◽  
Author(s):  
Guifang Zeng ◽  
Yongling An ◽  
Huifang Fei ◽  
Tian Yuan ◽  
Sun Qing ◽  
...  

In this work, nanosized polythiophene (PTh) is synthesized via a green and facile method. The obtained nanosized PTh was characterized by Fourier transform infrared (FTIR), X-ray diffraction (XRD), Brunauer–Emmett–Teller theory (BET) and scanning electron microscopy (SEM). The result indicated that a nanosized, porous and amorphous PTh was synthesized. As an organic anode material for potassium ion battery, the PTh shows excellent performance with a reversible capacity of 58[Formula: see text]mAh[Formula: see text]g[Formula: see text] at 30[Formula: see text]mA[Formula: see text]g[Formula: see text].


2020 ◽  
Vol 22 (2) ◽  
pp. 9-19 ◽  
Author(s):  
Fangping Li ◽  
Jun Zhang ◽  
Longjiang Wang ◽  
Weijian Liu ◽  
Qahtan A. Yousif

AbstractA green procedure for the one-pot three-component synthesis of 1-amidoalkyl-2-naphthol and 3-amino-1-phenyl-1H benzo[f]chromene-2-carbonitrile derivatives from the reaction of 2-naphtol, aldehydes, and malononitrile/acetamide in the presence of a catalytic amount of Fe3O4@enamine-B(OSO3H)2 as an efficient and novel heterogeneous magnetic nanostructure catalyst is described. The catalyst was characterized using Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), vibrating sample magnetometry (VSM), energy dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). These strategies possess some merits such as simple work-up method, easy preparation of the catalyst, short reaction times, good-to-high yields, and non-use of hazardous solvents during all steps of the reactions. Moreover, due to the magnetic nature of the catalyst, it was readily recovered by magnetic decantation and can be recycled at least six runs with no considerable decrease in catalytic activity.


2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Hui Ma ◽  
Qiang Gao ◽  
Chunxia Gao ◽  
Wei Bao ◽  
Mingqiao Ge

The electroconductive AZO@TiO2whiskers have been successfully preparedviacoating Al doped ZnO onto TiO2whisker. The orthogonal tests were employed to optimize the synthetic conditions. The crystallographic structure and the morphology of the AZO@TiO2whiskers and the polypropylene nonwoven fabrics modified with AZO@TiO2whiskers were characterized by X-ray photoelectron spectroscopy, X-ray diffraction, scanning electron microscope, four-probe meter, and electrometer. The results showed the AZO@TiO2whiskers exhibited good electroconductive performance. Moreover, the polypropylene nonwoven fabrics modified with AZO@TiO2whiskers revealed excellent antistatic performance indicating wide application of AZO@TiO2whiskers in the antistatic textiles.


2019 ◽  
Vol 45 ◽  
pp. 146867831982590
Author(s):  
Jiaojing Zhang ◽  
Hua Song ◽  
Yanguang Chen ◽  
Tianzhen Hao ◽  
Feng Li ◽  
...  

A series of APTMS ((3-aminopropyl)trimethoxysilane)-modified silicate MCM-41 adsorbents ( x-APTMS/MCM-41, x is the volume of APTMS per 1 g of silicate MCM-41) with different APTMS contents was prepared, and the effects of APTMS content on the desulfurization performance of the APTMS/MCM-41 adsorbents were studied in a fixed adsorption bed using H2S and N2 mixture as a model gas. The as-prepared adsorbents were characterized by X-ray diffraction analysis, N2 adsorption–desorption, Fourier transform infrared spectroscopy, transmission electron microscopy, scanning electron microscopy, and energy-dispersive spectroscopy. The results showed that all the APTMS-modified x-APTMS/MCM-41 adsorbents retained the mesoporous silica structure of MCM-41. The Brunauer–Emmett–Teller-specific surface area of x-APTMS/MCM-41 increased slightly with increasing x at first and then decreased with further increasing APTMS content. The H2S removal performances of x-APTMS/MCM-41 adsorbents decreased in the order 0.6-APTMS/MCM-41 > 0.7-APTMS/MCM-41 > 0.5-APTMS/MCM-41 > 0.4-APTMS/MCM-41 > 0.8-APTMS/MCM-41. At x = 0.6, the maximum H2S removal rate of 54.2% and H2S saturated capacity of 134.4 mg g−1 were observed. The regeneration experiment of 0.6-APTMS/MCM-41 adsorbent after three times regeneration at 423 K for 3 h in nitrogen confirmed that it possessed a good regenerability.


2022 ◽  
Vol 19 ◽  
Author(s):  
Runjhun Tandon ◽  
Shripad Patil ◽  
Nitin Tandon ◽  
Pushpendra Kumar

Abstract: A novel magnetite silica-coated nanoparticle-supported molybdate nanocatalyst has been prepared successfully by a simple co-precipitation method. Prepared nanocatalyst has been characterized by different techniques like Fourier Transmission Infrared Spectroscopy (FT-IR), X-ray diffraction (XRD), Field Emission Scanning Electron Microscope (FE-SEM) and Energy Dispersive X-ray Spectroscopy (EDX). Further, the catalytic activity of the nanocatalyst was explored for N-formylation reactions under solvent-free conditions. Interestingly, the catalyst could be reused for 10 cycles and only 2 mol % of the catalyst was sufficient to catalyze the N-formylation reaction at 700C under solvent-free conditions.


2012 ◽  
Vol 66 (7) ◽  
Author(s):  
Bahador Karami ◽  
Saeed Khodabakhshi ◽  
Zahra Haghighijou

AbstractTungstate sulfuric acid (TSA) was prepared, characterized, and applied for direct synthesis of novel and known benzimidazoles through a condensation reaction of o-phenylenediamines with orthoesters under solvent-free conditions. TSA was characterized by powdered X-ray diffraction (XRD), X-ray fluorescence (XRF), and FTIR spectroscopy. This novel and eco-friendly method is very cheap and has many advantages such as excellent yields, recyclable and eco-friendly catalyst, and simple work-up procedure.


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