scholarly journals Zn 1,3,5-benzenetricarboxylate as an efficient catalyst for the synthesis of cyclic carbonates from CO2

RSC Advances ◽  
2018 ◽  
Vol 8 (17) ◽  
pp. 9192-9201 ◽  
Author(s):  
Chao Feng ◽  
Xianglei Cao ◽  
Liugen Zhang ◽  
Changyan Guo ◽  
Naeem Akram ◽  
...  
Keyword(s):  
Heterogeneous Catalyst ◽  
Cycloaddition Reaction ◽  
Cyclic Carbonate ◽  
Solvent Free ◽  
Cyclic Carbonates ◽  
Efficient Catalyst ◽  
Solvent Free Conditions

[Zn3(BTC)2], a heterogeneous catalyst, can efficiently catalyze the cycloaddition reaction. Under relatively moderate and solvent-free conditions, the yield of cyclic carbonate reached 99%.

Nano-Polyoxotungstate as a Recyclable and Highly Efficient Catalyst for Cycloaddition of CO2 to Cyclic Carbonates under Solvent-free Conditions

2018 ◽  
Vol 15 (4) ◽  
pp. 533-540 ◽  
Author(s):  
Reza Haddad ◽  
Mehdi D. Telgerd ◽  
Hamid Abedi ◽  
Ali Roostaie
Keyword(s):  
Surface Acidity ◽  
Solvent Free ◽  
Cyclic Carbonates ◽  
Spent Catalyst ◽  
Efficient Catalyst ◽  
Filtration Method ◽  
External Magnet ◽  
Recoverable Catalyst ◽  
Solvent Free Conditions ◽  
Ft Ir

Aim and Objective: In this study, for the first time keplerate cluster [Cu20Cl(OH)24(H2O)12 (P8W48O184)]25- (hereafter [W48P8Cu20]) was supported on SMNP (Fe3O4-@SiO2) via amine functionality (ASMNP) as a magnetically-recoverable catalyst (hereafter [WPCu@ASMNP]). This nanocatalyst showed high activity for the synthesis of cyclic carbonates under solvent-free conditions. Materials and Methods: After preparation, the nanocatalyst was characterized by FT-IR, XRD, ICP-AES, TGA, TEM and SEM. Surface acidity was determined by a potentiometric titration with n-butyl amine. The effect of different parameters like catalyst amount, reaction time, temperature and pressure in the presence of [WPCu@ASMNP] were studied. Results: Optimal reaction conditions were obtained for 0.5mol% of catalyst, reaction temperature of 100°C and CO2 pressure of 1.5 MPa. The [WPCu@ASMNP] could be separated from the reaction and reused for five times with an external magnet without notable decrease in the activity. Finally, stability of the catalyst and its reusability were evaluated using a hot filtration method. The FT-IR and the control experiments (hot filtration) after five cycles confirmed the strongly catalyst immobilization to the ASMNP. Conclusion: The nanocatalyst is shown to be effective heterogeneous and recyclable catalyst for the synthesis of cyclic carbonates from CO2 and epoxides under mild conditions without any additional co-solvent and cocatalyst. This catalyst has a good substrate tolerance as demonstrated by its activity towards different epoxides. Importantly, the reaction could be carried out under solvent free conditions. The heterogeneous nature of the catalyst is proved by recovering and reusing this catalyst without any appreciable loss in catalytic activity and by the FT-IR spectroscopic characterization of the fresh and spent catalyst. The product separation and catalyst recycling are short using an external magnet.

Mesoporous Zirconium Oxophosphate: An Efficient Catalyst for the Synthesis of Cyclic Acetals and Cyclic Carbonates under Solvent-Free Conditions

2017 ◽  
Vol 2 (32) ◽  
pp. 10595-10602 ◽  
Author(s):  
Sk. Safikul Islam ◽  
Piyali Bhanja ◽  
Kajari Ghosh ◽  
Rostam Ali Molla ◽  
Nasima Yasmin ◽  
...  
Keyword(s):  
Solvent Free ◽  
Cyclic Carbonates ◽  
Efficient Catalyst ◽  
Cyclic Acetals ◽  
Solvent Free Conditions

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 Highly Efficient MOF Catalyst Systems for CO2 Conversion to Bis-Cyclic Carbonates as Building Blocks for NIPHUs (Non-Isocyanate Polyhydroxyurethanes) Synthesis

Catalysts ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 628
Author(s):  
Adolfo Benedito ◽  
Eider Acarreta ◽  
Enrique Giménez
Keyword(s):  
Molar Mass ◽  
Cycloaddition Reaction ◽  
Building Blocks ◽  
Catalyst System ◽  
Cyclic Carbonate ◽  
Ammonium Bromide ◽  
Cyclic Carbonates ◽  
High Molar Mass ◽  
Highly Efficient ◽  
Free Process

The present paper describes a greener sustainable route toward the synthesis of NIPHUs. We report a highly efficient solvent-free process to produce [4,4′-bi(1,3-dioxolane)]-2,2′-dione (BDC), involving CO2, as renewable feedstock, and bis-epoxide (1,3-butadiendiepoxide) using only metal–organic frameworks (MOFs) as catalysts and cetyltrimethyl-ammonium bromide (CTAB) as a co-catalyst. This synthetic procedure is evaluated in the context of reducing global emissions of waste CO2 and converting CO2 into useful chemical feedstocks. The reaction was carried out in a pressurized reactor at pressures of 30 bars and controlled temperatures of around 120–130 °C. This study examines how reaction parameters such as catalyst used, temperature, or reaction time can influence the molar mass, yield, or reactivity of BDC. High BDC reactivity is essential for producing high molar mass linear non-isocyanate polyhydroxyurethane (NIPHU) via melt-phase polyaddition with aliphatic diamines. The optimized Al-OH-fumarate catalyst system described in this paper exhibited a 78% GC-MS conversion for the desired cyclic carbonates, in the absence of a solvent and a 50 wt % chemically fixed CO2. The cycloaddition reaction could also be carried out in the absence of CTAB, although lower cyclic carbonate yields were observed.

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