Nickel (II) and oxovanadium (IV) complexes supported on MCM-41 mesoporous and their application in catalytic selective sulfide and thiol oxidation

Author(s):  
Mohsen Nikoorazm ◽  
Maryam Khanmoradi ◽  
Masoumeh Sayadian

Introduction:: MCM-41 was synthesized using the sol-gel method. Then two new transition metal complexes of Nickel (II) and Vanadium (IV), were synthesized by immobilization of adenine (6-aminopurine) into MCM-41 mesoporous. The compounds have been characterized by XRD, TGA, SEM, AAS and FT-IR spectral studies. Using these catalysts provided an efficient and enantioselective procedure for oxidation of sulfides to sulfoxides and oxidative coupling of thiols to their corresponding disulfides using hydrogen peroxide at room temperature. Materials and Methods:: To a solution of sulfide or thiol (1 mmol) and H2O2 (5 mmol), a determined amount of the catalyst was added. The reaction mixture was stirred at room temperature for the specific time under solvent free conditions. The progress of the reaction was monitored by TLC using n-hexane: acetone (8:2). Afterwards, the catalyst was removed from the reaction mixture by centrifugation and, then, washed with dichloromethane in order to give the pure products. Results:: All the products were obtained in excellent yields and short reaction times indicating the high activity of the synthesized catalysts. Besides, the catalysts can be recovered and reused for several runs without significant loss in their catalytic activity. Conclusion:: These catalytic systems furnish the products very quickly with excellent yields and VO-6AP-MCM-41 shows high catalytic activity compared to Ni-6AP-MCM-41.

2018 ◽  
Vol 21 (8) ◽  
pp. 602-608 ◽  
Author(s):  
Zainab Ehsani-Nasab ◽  
Ali Ezabadi

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 ◽  
2019 ◽  
Vol 51 (23) ◽  
pp. 4487-4497
Author(s):  
Gan Jiang ◽  
Yang Lin ◽  
Mingzhong Cai ◽  
Hong Zhao

The heterogeneous copper(II)-catalyzed oxidative cyclization of 2-pyridine ketone hydrazones was achieved in ethyl acetate at room temperature in the presence of an MCM-41-anchored bidentate 2-aminoethylamino copper(II) catalyst [MCM-41-2N-Cu(OAc)2], in the presence of air as the oxidant, yielding a wide variety of [1,2,3]triazolo[1,5-a]pyridines in mostly good to high yields. The present method was also applied to the direct one-pot synthesis of [1,2,3]triazolo[1,5-a]pyridines from 2-acylpyridine derivatives and hydrazine monohydrate. Importantly, this supported copper(II) catalyst could be conveniently obtained via a simple procedure from easily available and inexpensive reagents, recovered by filtration of the reaction mixture, and reused at least seven times without a significant loss of catalytic activity.


2016 ◽  
Vol 6 (3) ◽  
pp. 869-874 ◽  
Author(s):  
Shu-Tao Gao ◽  
Weihua Liu ◽  
Cheng Feng ◽  
Ning-Zhao Shang ◽  
Chun Wang

Ag–Pd alloys deposited on an amine-functionalized UiO-66(NH2–UiO-66) have been successfully prepared via a pre-coordination method and used as a AgPd@NH2–UiO-66 catalyst with 100% H2 selectivity and a high catalytic activity.


2016 ◽  
Vol 09 (06) ◽  
pp. 1642009 ◽  
Author(s):  
Jing Zhou ◽  
Yong Zhao ◽  
Lifan Qin ◽  
Chen Zeng ◽  
Wei Xiao

Uniform CoSn(OH)6 hollow nanoboxes and the derivative with Pt loading (Pt/CoSn(OH)6) were herein synthesized and characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). SEM and TEM analyses showed that CoSn(OH)6 possessed mesoporous hollow structure and Pt nanoparticles with size of 2–8[Formula: see text]nm were uniformly dispersed on the surface of CoSn(OH)6 nanoboxes. The performances of the catalysts for the formaldehyde (HCHO) removal at room temperature were evaluated. These Pt/CoSn(OH)6 catalysts exhibited a remarkable catalytic activity as well as stability for room-temperature oxidative decomposition of gaseous HCHO, while the corresponding CoSn(OH)6 only showed adsorption. The synergetic effect between the highly dispersed Pt nanoparticles and the CoSn(OH)6 nanoboxes with mesoporous hollow structure, a large surface area and abundant surface hydroxyl groups is considered to be the main reason for the observed high catalytic activity of Pt/CoSn(OH)6.


Catalysts ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 252 ◽  
Author(s):  
Gabriela Dobras ◽  
Kornela Kasperczyk ◽  
Sebastian Jurczyk ◽  
Beata Orlińska

N-Hydroxyphthalimide was immobilized via ester bond on commercially available silica gel (SiOCONHPI) and then coated with various ionic liquids containing dissolved CoCl2 (SiOCONHPI@CoCl2@IL). New catalysts were characterized by means of FT IR spectroscopy, elemental analysis, SEM and TGA analysis and used in ethylbenzene oxidation with oxygen under mild solvent-free conditions (80 °C, 0.1 MPa). High catalytic activity of SiOCONHPI was proved. In comparison to a non-catalytic reaction, a two-fold increase in conversion of ethylbenzene was observed (from 4.7% to 8.6%). Coating of SiOCONHPI with [bmim][OcOSO3], [bmim][Cl] and [bmim][CF3SO3] containing CoCl2 enabled to increase the catalytic activity in relation to systems in which IL and CoCl2 were added directly to reaction mixture. The highest conversion of ethylbenzene was obtained while SiOCONHPI@CoCl2@[bmim][OcOSO3] were used (12.1%). Catalysts recovery and reuse was also studied.


2019 ◽  
Vol 31 (10) ◽  
pp. 2181-2184
Author(s):  
Abdulrahman I. Alharthi

The effect of calcination on the performance of tungstophosphoric acid for the product of Knoevenagel condensation was investigated. Substituted aldehydes and dimedone has been used in the presence of calcined tungstophosphoric acid as a heterogeneous catalyst using grinding method at room temperature. The results of reactions revealed that calcined tungstophosphoric acid has superior catalytic activity comparing to non-calcined catalyst in terms of yield and reaction time. Maximum yield of model compound was achieved by using 10 mol% of calcined catalyst in a reaction time that does not exceed 10 min, whereas the yield at same amount of non-calcined catalyst was 86 % in a reaction time of 35 min.


2001 ◽  
Vol 56 (3) ◽  
pp. 263-270 ◽  
Author(s):  
Veli T. Kasumov

Abstract Several new binuclear nickel(II), oxovanadium(IV) and palladium(II) complexes (MLX) of tridentate salicylaldimines (LXH2) obtained from substituted salicylaldehydes and 2,4-di-tert-butyl-6-aminophenol, as well as mononuclear nickel(II) and oxovanadium(IV), MQx nH2O, complexes with hydrogenated LX H2 ligands (QXH2) have been prepared and their spectroscopic, magnetic and catalytic activity (for PdLx) have been investigated. NiLx and VOLx complexes when dissolved in pyridine, take up three or two pyridine molecules to form six coordinated complexes, respectively. The Ni(II) and VO(IV) complexes obtained from QXH2 can be formu­lated as NiQx-3H2O and VOQx H2O. All VO(IV) complexes have been characterized by ESR parameters. It has been found that some PdLx complexes without any preliminary activation, in EtOH, THF and DMF exhibit high catalytic activity in the hydrogenation of nitrobenzene or cyclohexene at room temperature and at 30 -40 °C under 760 torr H2. When this reaction has been carried out in the ESR cavity at room temperature the triplet of 12 line multiplets due to the nitroxyl type coordinated radical (g = 2.013, AN = 10 G, AH = 0.8 G) was detected.


2014 ◽  
Vol 1025-1026 ◽  
pp. 621-627
Author(s):  
Qin Mei Peng ◽  
Bo Li ◽  
Jin Wang ◽  
Ji Jiao Li ◽  
Ji Zhou

Three-dimensional (3-D) periodic hematite scaffold was successfully fabricated by direct writing method as a catalyst for degradation of organic contaminants. Photo-catalytically active α-Fe2O3 nanoparticles have been synthesized by sol-gel technique. Aqueous slurries of iron oxides were freeform fabricated to produce hematite scaffolds with a 3-D periodic architecture and multiscale porosity. The catalytic activity of the hematite scaffolds was evaluated in the degradation of Methylene Blue (MB). It was found that the degradation rate of MB dye was over 83%. The result strongly indicates that the hematite scaffolds exhibits a high catalytic activity. Moreover, this work provides an important step forward in the creation of suitable structures for photocatalyst.


2012 ◽  
Vol 90 (3) ◽  
pp. 290-297 ◽  
Author(s):  
Manoj Kumar Muthyala ◽  
Bhupender S Chhikara ◽  
Keykavous Parang ◽  
Anil Kumar

A novel ionic-liquid-supported 1,5,7-triazabicyclo[4.4.0]dec-5-ene (IL–TBD) was synthesized and investigated for its ability to act as an active organocatalyst in the Michael addition of active methylene compounds and thiophenols to chalcones under solvent-free conditions. The IL–TBD afforded Michael addition products in excellent yields (82%–94%) at room temperature, and it was simply recycled and reused at least five times without significant loss of catalytic activity.


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