Synthesized NaA nanozeolite as a catalyst for the preparation of 3-amino imidazo[1,2-a]pyridines under solvent-free conditions

2021 ◽  
Vol 19 ◽  
Author(s):  
Sara Azargashb ◽  
Afshin Sarvary ◽  
Seyed Karim Hassaninejad-Darzi
Keyword(s):  
Synthesis Method ◽  
Total Pore Volume ◽  
Particle Size Analysis ◽  
Solvent Free ◽  
Bet Surface Area ◽  
Size Analysis ◽  
X Ray Diffraction ◽  
Efficient Catalyst ◽  
Solvent Free Conditions ◽  
Recycle And Reuse

Abstract: The present study explores a new method for the fabrication of NaA nanozeolite as a simple and efficient catalyst for the production of 3-aminoimidazo [1,2-a] pyridines through the 3-component reaction of aldehydes, 2-aminoperidines and isocyanides under solvent-free conditions. The production of organic template free (OTF) NaA nanozeolite was performed at room temperature. The prepared nanozeolite was identified by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electronic microscopy (FESEM), N2 sorption isotherm and particle size analysis (PSA). The particle sizes of synthesized spherical NaA nanozeolite were under 100 nm via the FESEM method. The BET surface area, total pore volume and mean pore diameter of the created sample were attained to be 362 m2g-1, 0.44 cm3 g-1 and 5.9 nm, respectively. The developed method has some advantages such as OTF production of NaA nanozeolite, simple synthesis method with short reaction time and easy separation using filtration and the ability to recycle and reuse of catalyst several times without reducing its efficiency.

Mechano-chemical effects on surface properties and molybdate exchange on hydrotalcite

Clay Minerals ◽  
2009 ◽  
Vol 44 (3) ◽  
pp. 311-317 ◽  
Author(s):  
J. Bonifacio-Martínez ◽  
J. Serrano-Gómez ◽  
Ma. Del Carmen López-Reyes ◽  
F. Granados-Correa
Keyword(s):  
Particle Size ◽  
Total Pore Volume ◽  
Specific Area ◽  
Surface Characteristics ◽  
Particle Size Analysis ◽  
Size Analysis ◽  
X Ray Diffraction ◽  
Ion Content ◽  
X Ray ◽  
Chemical Effects

AbstractThe effects of mechano-chemical treatment on the surface characteristics and sorption properties of hydrotalcite were studied. Non-milled (crushed) and milled samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), particle size analysis and specific area. A milling time of 2 h decreased the particle size of the hydrotalcite samples from 21 to 8.0 nm, the specific area from 97 to 5.7 m2 g–1 and the total pore volume from 0.41 to 0.01 cm3. After the crushed and milled samples had been separately calcined at 500ºC, they were agitated with 10–2 M Na2MoO4 aqueous solutions for 48 h. The molybdate ion content in the regenerated non-milled hydrotalcite samples (HTc-MoO4) was found to be 6.0 meq g–1 while in the milled hydrotalcite (HTm-MoO4) samples this content was 2.5 meq g–1. The lower molybdate content was thought to be a result of compaction and, hence, reduced reactivity of the milled HT samples.

Copper Oxide Nanoparticles as a Mild and Efficient Catalyst for N-Arylation of Imidazole and Aniline with Boronic Acids at Room Temperature

Synlett ◽  
2017 ◽  
Vol 28 (10) ◽  
pp. 1177-1182 ◽  
Author(s):  
Ashim Thakur ◽  
Raju Borah ◽  
Prasanta Raul ◽  
Abhijit Mahanta ◽  
Andrey Shchukarev ◽  
...  
Keyword(s):  
Surface Area ◽  
Room Temperature ◽  
Copper Oxide Nanoparticles ◽  
Particle Size Analysis ◽  
Significant Loss ◽  
Bet Surface Area ◽  
Size Analysis ◽  
Oxide Nanoparticles ◽  
Efficient Catalyst ◽  
Ft Ir

The present work describes the excellent catalytic activity of copper(II) oxide nanoparticles (NPs) towards N-arylation of aniline and imidazole at room temperature. The copper(II)oxide NPs were synthesized by a thermal refluxing technique and characterized by FT-IR spectroscopy; powder XRD, SEM, EDX, TEM, TGA, XPS, BET surface area analysis, and particle size analysis. The size of the NPs was found to be around 12 nm having a surface area of 164.180 m2 g–1.The catalytic system was also found to be recyclable and could be reused in subsequent catalytic runs without a significant loss of activity.

Preparation and Characterization of a Novel Room Temperature Dicationic Ionic Liquid and its Application in the Synthesis of Xanthenediones Under Solvent-Free Conditions

2018 ◽  
Vol 21 (8) ◽  
pp. 602-608 ◽  
Author(s):  
Zainab Ehsani-Nasab ◽  
Ali Ezabadi
Keyword(s):  
Ionic Liquid ◽  
Room Temperature ◽  
Reaction Times ◽  
Significant Loss ◽  
Solvent Free ◽  
Acidity Function ◽  
Efficient Catalyst ◽  
Solvent Free Conditions ◽  
Hammett Acidity Function ◽  
Dicationic Ionic Liquid

Aim and Objective: In the present work, 1, 1’-sulfinyldiethylammonium bis (hydrogen sulfate) as a novel room temperature dicationic ionic liquid was synthesized and used as a catalyst for xanthenediones synthesis. Material and Method: The dicationic ionic liquid has been synthesized using ethylamine and thionyl chloride as precursors. Then, by the reaction of [(EtNH2)2SO]Cl2 with H2SO4, [(EtNH2)2SO][HSO4]2 was prepared and after that, it was characterized by FT-IR, 1H NMR, 13C NMR as well as Hammett acidity function. This dicationic ionic liquid was used as a catalyst for the synthesis of xanthenediones via condensation of structurally diverse aldehydes and dimedone under solvent-free conditions. The progress of the reaction was monitored by thin layer chromatography (ethyl acetate/n-hexane = 3/7). Results: An efficient solvent-free method for the synthesis of xanthenediones has been developed in the presence of [(EtNH2)2SO][HSO4]2 as a powerful catalyst with high to excellent yields, and short reaction times. Additionally, recycling studies have demonstrated that the dicationic ionic liquid can be readily recovered and reused at least four times without significant loss of its catalytic activity. Conclusion: This new dicationic ionic liquid can act as a highly efficient catalyst for xanthenediones synthesis under solvent-free conditions.

Synthesis of Dihydropyrimidinones (DHPMs) and Hexahydro Xanthene Catalyzed by 1,4-Diazabicyclo [2.2.2] Octane Triflate Under Solvent-Free Condition

2019 ◽  
Vol 16 (5) ◽  
pp. 776-786 ◽  
Author(s):  
Deepa ◽  
Geeta D. Yadav ◽  
Mohd J. Aalam ◽  
Pooja Chaudhary ◽  
Surendra Singh
Keyword(s):  
Ethyl Acetoacetate ◽  
Biginelli Reaction ◽  
Solvent Free ◽  
Efficient Catalyst ◽  
Solvent Free Condition ◽  
Solvent Free Conditions ◽  
Xanthene Derivatives ◽  
Different Temperatures ◽  
Flash Column Chromatography ◽  
Biginelli Condensation

Objective:DABCO salts were evaluated as catalysts for the Biginelli reaction between 4- methoxybenzaldehyde, urea and ethyl acetoacetate under solvent-free conditions. 1,4-Diazabicyclo [2.2.2] octane triflate was found to be a simple, inexpensive, highly efficient catalyst for Biginelli reaction for a variety aromatic aldehyde with urea and ethyl acetoacetate at 80°C afforded corresponding 3,4-dihydropyrimidinones in 50-99% yields after 30-120 minutes. 1,3-Cyclohexadione was used in place of ethyl acetoacetate in the absence of urea this methodology is giving hexahydro xanthene derivatives in good to excellent yields after 3-4 hours.Methods:DABCO salt 4 (5 mol%), 4-methoxybenzaldehyde (0.73 mmol) and urea (0.73 mmol) were stirred for 10 minutes at 80°C, then ethyl acetoacetate (1.5 equiv.) was added and reaction mixture was stirred at 80°C for specified time. The resulting solution was stirred continuously and progress of the reaction was followed by TLC. The crude reaction mixture was purified by flash column chromatography on silica gel (hexane/ethyl acetate (1:2)) to give pure desired product.Results:Reaction conditions of the Biginelli reaction were optimized using 4-methoxybenzaldehyde (0.73 mmol), urea (0.73 mmol), and ethyl acetoacetate (5 equiv.) as model substrates catalyzed by 1,4-Diazabicyclo [2.2.2] octane triflate (5 mol%) in a different solvents, screening of different catalysts and different temperatures. Neat condition was found to be the best for the Biginelli condensation and corresponding 3,4- dihydropyrimidinones was obtained in good to excellent yields. When the reaction was carried out with benzaldehyde derivatives and cyclohexane-1,3-dione in place of ethyl acetoacetate in the absence of urea, solely corresponding hexahydro xanthene derivatives were obtained in 61-91% yields.Conclusion:In conclusion, we have applied salts of 1,4-Diaza-bicyclo [2.2.2] octane as catalysts in the Biginelli condensation and corresponding 3,4-dihydropyrimidinones were obtained in 50- 99% yields under solvent free conditions. This methodology is having advantages like simple work-up; low loading of catalyst and reaction was performed at moderate temperature under solvent-free conditions.

scholarly journals Mining Wastes of an Albite Deposit as Raw Materials for Vitrified Mullite Ceramics

Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 232
Author(s):  
Pedro J. Sánchez-Soto ◽  
Eduardo Garzón ◽  
Luis Pérez-Villarejo ◽  
George N. Angelopoulos ◽  
Dolores Eliche-Quesada
Keyword(s):  
Particle Size ◽  
Raw Materials ◽  
Phase Evolution ◽  
Particle Size Analysis ◽  
Size Analysis ◽  
Mining Wastes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Maximum Value

In this work, an examination of mining wastes of an albite deposit in south Spain was carried out using X-ray Fluorescence (XRF), X-ray diffraction (XRD), particle size analysis, thermo-dilatometry and Differential Thermal Analysis (DTA) and Thermogravimetric (TG) analysis, followed by the determination of the main ceramic properties. The albite content in two selected samples was high (65–40 wt. %), accompanied by quartz (25–40 wt. %) and other minor minerals identified by XRD, mainly kaolinite, in agreement with the high content of silica and alumina determined by XRF. The content of Na2O was in the range 5.44–3.09 wt. %, being associated with albite. The iron content was very low (<0.75 wt. %). The kaolinite content in the waste was estimated from ~8 to 32 wt. %. The particle size analysis indicated values of 11–31 wt. % of particles <63 µm. The ceramic properties of fired samples (1000–1350 °C) showed progressive shrinkage by the thermal effect, with water absorption and open porosity almost at zero at 1200–1250 °C. At 1200 °C, the bulk density reached a maximum value of 2.38 g/cm3. An abrupt change in the phase evolution by XRD was found from 1150 to 1200 °C, with the disappearance of albite by melting in accordance with the predictions of the phase diagram SiO2-Al2O3-Na2O and the system albite-quartz. These fired materials contained as main crystalline phases quartz and mullite. Quartz was present in the raw samples and mullite was formed by decomposition of kaolinite. The observation of mullite forming needle-shape crystals was revealed by Scanning Electron Microscopy (SEM). The formation of fully densified and vitrified mullite materials by firing treatments was demonstrated.

scholarly journals Development of a Solid Dispersion of Nystatin with Maltodextrin as a Carrier Agent: Improvements in Antifungal Efficacy against Candida spp. Biofilm Infections

2021 ◽  
Vol 14 (5) ◽  
pp. 397
Author(s):  
Carlos Benavent ◽  
Carlos Torrado-Salmerón ◽  
Santiago Torrado-Santiago
Keyword(s):  
Antifungal Activity ◽  
Solid Dispersions ◽  
Particle Size Analysis ◽  
Size Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Candida Spp ◽  
Microbiological Techniques ◽  
Characterization Studies ◽  
Candida Albicans Biofilms

The aim of this study was to improve the treatment of Candida albicans biofilms through the use of nystatin solid dispersions developed using maltodextrins as a hyperosmotic carrier. Characterization studies by differential scanning calorimetry, X-ray diffraction, dissolution studies, and particle size analysis were performed to evaluate changes in nystatin crystallinity. Antifungal activity and anti-biofilm efficacy were assessed by microbiological techniques. The results for nystatin solid dispersions showed that the enhancement of antifungal activity may be related to the high proportions of maltodextrins. Anti-biofilm assays showed a significant reduction (more than 80%) on biofilm formation with SD-N:MD [1:6] compared to the nystatin reference suspension. The elaboration process and physicochemical properties of SD-N:MD [1:6] could be a promising strategy for treatment of Candida biofilms.

Preparation of xanthated bentonite and its removal behavior for Pb(II) ions

2010 ◽  
Vol 61 (5) ◽  
pp. 1235-1243 ◽  
Author(s):  
Y. F. He ◽  
F. R. Li ◽  
R. M. Wang ◽  
F. Y. Li ◽  
Y. Wang ◽  
...  
Keyword(s):  
Adsorption Mechanism ◽  
Removal Rate ◽  
Freundlich Isotherm ◽  
Particle Size Analysis ◽  
Lead Ions ◽  
Size Analysis ◽  
Optimum Conditions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir

Xanthate was successfully grafted onto bentonite by a relatively simple solution reaction. The obtained xanthated bentonite (XBent) was characterized by FT-IR spectrophotometer, thermogravimetric analysis (TG), particle size analysis, x-ray diffraction (XRD) and scanning electron microscopy (SEM). XBent acting as a type of environmentally friendly adsorbent was applied to remove lead ions from aqueous solutions. The optimum conditions were as follows: [Pb2 + ] = 500 mg L−1, [XBent] = 2 g L−1, pH = 5.0; oscillating 60 min under 200 rpm at 25°C. The removal rate of lead was up to 99.9%. It was found that the lead(II) ions—XBent adsorption isotherm model fitted well to the Freundlich isotherm. The adsorption mechanism was also investigated by SEM and XRD, which concluded that lead ions were complexed or chelated with XBent. XBent appears to have potential to be used later in water treatment as a type of inorganic polymer reagent.

Synthesis of Alpha-Tricalcium Phosphate by Wet Reaction and Evaluation of Mechanical Properties

2012 ◽  
Vol 727-728 ◽  
pp. 1164-1169 ◽  
Author(s):  
Mônica Beatriz Thürmer ◽  
Rafaela Silveira Vieira ◽  
Juliana Machado Fernandes ◽  
Wilbur Trajano Guerin Coelho ◽  
Luis Alberto Santos
Keyword(s):  
Mechanical Properties ◽  
Calcium Phosphate ◽  
Tricalcium Phosphate ◽  
Calcium Nitrate ◽  
Chemical Precipitation ◽  
Particle Size Analysis ◽  
Size Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Calcium Phosphate Cements

Calcium phosphate cements have bioactivity and osteoconductivity and can be molded and replace portions of bone tissue. The aim of this work was to study the obtainment of α-tricalcium phosphate, the main phase of calcium phosphate cement, by wet reaction from calcium nitrate and phosphoric acid. There are no reports about α-tricalcium phosphate obtained by this method. Two routes of chemical precipitation were evaluated and the use of two calcinations temperatures to obtain the phase of cement. The influence of calcination temperature on the mechanical properties of cement was evaluated. Cement samples were characterized by particle size analysis, X-ray diffraction, mechanical strength and scanning electron microscopy. The results demonstrate the strong influence of synthesis route on the crystalline phases of cement and the influence of concentration of reactants on the product of the reaction, as well as, on the mechanical properties of cement.

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