Search results for: solvothermal synthesis

Authors: Jafar Akbari

Abstract:

Quinolines are very important compounds partially because of their pharmacological properties which include wide applications in medicinal chemistry. notable among them are antimalarial drugs, anti-inflammatory agents, antiasthamatic, antibacterial, antihypertensive, and tyrosine kinase inhibiting agents. Despite quinoline usage in pharmaceutical and other industries, comparatively few methods for their preparation have been reported.The Friedlander annulation is one of the simplest and most straightforward methods for the synthesis of poly substituted quinolines. Although, modified methods employing lewis or br¢nsted acids have been reported for the synthesis of quinolines, the development of water stable acidic catalyst for quinoline synthesis is quite desirable. One of the most remarkable features of ionic liquids is that the yields can be optimized by changing the anions or the cations. Recently, sulfonic acid functionalized ionic liquids were used as solvent-catalyst for several organic reactions. We herein report the one pot domino approach for the synthesis of quinoline derivatives in Friedlander manner using TSIL as a catalyst. These ILs are miscible in water, and their homogeneous system is readily separated from the reaction product, combining advantages of both homogeneous and heterogeneous catalysis. In this reaction, the catalyst plays a dual role; it ensures an effective condensation and cyclization of 2-aminoaryl ketone with second carbonyl group and it also promotes the aromatization to the final product. Various types of quinolines from 2-aminoaryl ketones and β-ketoesters/ketones were prepared in 85-98% yields using the catalytic system of SO3-H functionalized ionic liquid/H2O. More importantly, the catalyst could be easily recycled for five times without loss of much activity.

Keywords: antimalarial drugs, green chemistry, ionic liquid, quinolines

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Authors: Aida Safiera, Andika Dwi Rubyantoro, Muhammad Bagus Prakasa

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Indonesia’s needs of diesel oil each year are increasing and getting urge. However, that problems are not supported by the amount of oil production that still low and also influenced by the fact of oil reserve is reduced. Because of that, the government prefers to import from other countries than fulfill the needs of diesel. To anticipate that problem, development of fuel based on renewable diesel is started. Renewable diesel is renewable alternative fuel that is hydrocarbon derivative from decarbonylation of non-edible oil. Indonesia is rich with natural resources, including nyamplung oil (Calophyllum inophyllum oil) and zeolite. Nyamplung oil (Calophyllum inophyllum oil) has many stearic acids which are useful on renewable diesel synthesis meanwhile zeolite is cheap. Zeolite is many used on high temperature reaction and cracking process on oil industry. Zeolite also has advantages which are a high crystallization, surface area and pores. In this research, the main focus that becomes our attention is on preparation and characterization of metal nanocrystal. Active site that used in this research is Nickel Molybdenum (NiMo). The advantage of nanocrystal with nano scale is having larger surface area. The synthesis of metal nanocrystal will be done with conventional preparation modification method that is called simple heating. Simple heating method is a metal nanocrystal synthesis method using continuous media which is polymer liquid. This method is a simple method and produces a small particles size in a short time. Influence of metal nanocrystal growth on this method is the heating profile. On the synthesis of nanocrystal, the manipulated variables are temperature and calcination time. Results to achieve from this research are diameter size on nano scale (< 100 nm) and uniform size without any agglomeration. Besides that, the conversion of synthesis of renewable diesel is high and has an equal specification with petroleum diesel. Catalyst activities are tested by FT-IR and GC-TCD on decarbonylation process with a pressure 15 bar and temperature 375 °C. The highest conversion from this reaction is 35% with selectivity around 43%.

Keywords: renewable diesel, simple heating, metal nanocrystal, NiMo, zeolite

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Authors: R. Yuvakkumar, S. I. Hong

Abstract:

Visible light driven monoclinic α-Bi2O3 photocatalyst was synthesized employing green synthesis method using rambutan peel wastes. 10 ml rambutan extract was added to 50 ml of 0.1M Bi(NO3)3 under stirring at about 80°C for 2 hours. The centrifuged and dried product was calcinated in a muffle furnace at 450°C to get pure α-Bi2O3. The characterized product photocatalytic activity was evaluated employing methyl orange (MeO) as model pollutant with 10 mg l-1 concentration at pH 7. The obtained product optical absorption edges located at 484 nm clearly revealed the photocatalyst excitation by visible light irradiation. The obtained yellow color photocatalyst accord with its strong absorption spectrum revealed the visible light absorption due to the band gap transition. The band gap energy of α-Bi2O3 was estimated to be 2.81 eV indicating the absorption of α-Bi2O3 in visible light region. The photocatalytic results of MeO degradation revealed that green synthesized Bi2O3 can effectively degrade 92% MeO within 240 min under visible light (>400 nm), which is slightly increased to that of chemically synthesized Bi2O3 (90%).

Keywords: green synthesis, bismuth oxide, photocatalytic activity, nano

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Authors: Indah Kurniawaty, Yoki Yulizar, Haryo Satriya Oktaviano, Adam Kusuma Rianto

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Magnesium oxide nanoparticles (MgO NP) were successfully synthesized in this study using a one-pot green synthesis mediated by Calliandra Calothyrsus leaf extract (CLE). CLE was prepared by maceration of the leaf using methanol with a ratio of 1:5 for 7 days. Secondary metabolites in CLE, such as alkaloids and flavonoids, served as a weak base provider and capping agent in the formation of MgO NP. CLE Fourier Transform Infra-Red (FTIR) spectra peak at 3255, 1600, 1384, 1205, 1041, and 667 cm-1 showing the presence of vibrations O-H stretching, N-H bending, C-C stretching, C-N stretching and N-H wagging. During the experiment, different CLE volumes and calcined temperatures were used, resulting in a variety of structures. Energy Dispersive X-ray Spectrometer (EDS) and FTIR were used to characterize metal oxide particles. MgO diffraction pattern at 2θ of 36.9°; 42.9°; 62.2°; 74.6°; and 78.5° which can be assigned to crystal planes (111), (200), (220), (311), and (222), respectively. Scanning Electron Microscopy (SEM) was used to characterize the surface morphology. The morphology ranged from sphere to flower-like resulting in crystallite sizes of 28, 23, 12, and 9 nm.

Keywords: MgO, nanoparticle, calliandra calothyrsus, green-synthesis

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Authors: Waleed A. El-Said, Dina M. Fouad, Mohamed H. Aly, Mohamed A. El-Gahami

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Green synthesis of nanomaterials has received increasing attention as an eco-friendly technology in materials science. Here, we have used two types of extractions from green tea leaf (i.e. total extraction and tannin extraction) as reducing agents for a rapid, simple and one step synthesis method of mesoporous silica nanoparticles (MSNPs)/iron oxide (Fe3O4) nanocomposite based on deposition of Fe3O4 onto MSNPs. MSNPs/Fe3O4 nanocomposite were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray, vibrating sample magnetometer, N2 adsorption, and high-resolution transmission electron microscopy. The average mesoporous silica particle diameter was found to be around 30 nm with high surface area (818 m2/gm). MSNPs/Fe3O4 nanocomposite was used for removing lindane pesticide (an environmental hazard material) from aqueous solutions. Fourier transform infrared, UV-vis, High-performance liquid chromatography and gas chromatography techniques were used to confirm the high ability of MSNPs/Fe3O4 nanocomposite for sensing and capture of lindane molecules with high sorption capacity (more than 89%) that could develop a new eco-friendly strategy for detection and removing of pesticide and as a promising material for water treatment application.

Keywords: green synthesis, mesoporous silica, magnetic iron oxide NPs, adsorption Lindane

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Authors: Delele Worku Ayele, Bing-Joe Hwang

Abstract:

A method that does not employ hot injection techniques has been developed for the size-tunable synthesis of high-quality CdSe quantum dots (QDs) with a zinc blende structure. In this environmentally benign synthetic route, which uses relatively less toxic precursors, solvents, and capping ligands, CdSe QDs that absorb visible light are obtained. The size of the as-prepared CdSe QDs and, thus, their optical properties can be manipulated by changing the microwave reaction conditions. The QDs are characterized by XRD, TEM, UV-vis, FTIR, time-resolved fluorescence spectroscopy, and fluorescence spectrophotometry. In this approach, the reaction is conducted in open air and at a much lower temperature than in hot injection techniques. The use of microwaves in this process allows for a highly reproducible and effective synthesis protocol that is fully adaptable for mass production and can be easily employed to synthesize a variety of semiconductor QDs with the desired properties. The possible application of the as-prepared CdSe QDs has been also assessed using deposition on TiO2 films.

Keywords: average life time, CdSe QDs, microwave (MW), mass production oleic acid, Na2SeSO3

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Deivasigamani Ranjith Kumar, Jae-Jin Shim

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The quest for alternative sources of energy storage had led to the exploration on supercapacitors. Hybrid supercapacitors, a combination of carbon-based material and transition metals, had yielded long and improved cycle life as well as high energy and power densities. In this study, microwave irradiation was used for the facile and rapid synthesis of mesoporous RGO@(Co,Mn)3O4 nanosheets as an active electrode material. The advantages of this method include the non-use of reducing agents and acidic medium, and no further post-heat treatment. Additionally, it offers shorter reaction time at low temperature and low power requirement, which allows low fabrication and energy cost. The as-prepared electrode material demonstrated a high capacitance of 953 F•g−1 at 1 A•g−1 in a 6 M KOH electrolyte. Furthermore, the electrode exhibited a high energy density of 76.2 Wh•kg−1 (power density of 720 W•kg−1) and a high power density of 7200 W•kg−1 (energy density of 38 Wh•kg−1). The successful synthesis was considered to be efficient and cost-effective, with very promising electrochemical performance that can be used as an active material in supercapacitors.

Keywords: cobalt manganese oxide, electrochemical, graphene, microwave synthesis, supercapacitor

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Authors: J. Morillo, Otal E., A. Caballero, R. M. Pereñiguez, J. Usero

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The present work shows in the first place, the manufacture of the perovskitic material used as adsorbent, by means of two different methods to obtain two types of perovskites (LaFeO₃ and BiFeO₃). The results of this work show the characteristics of this manufactured material, as well as the synthesis yields obtained, achieving a better result for the self-combustion synthesis. Secondly, from the manufactured perovskites, an adsorption system has been developed, at the laboratory level, for the adsorption of the emerging pollutants Trimethoprim, Ciprofloxacin and Ibuprofen.

Keywords: nanostructured materials, emerging pollutants, water, adsorption processes

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Authors: Jinjoo Jung, Hayeon Won, Doyeong Jeong, Do Hyung Kim

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We present the electrochemical and electrochromic performance of the novel crystalline tungsten oxide and tungsten-molybdenum oxide nanostructures synthesized by utilizing solvo-thermal method with hexacarbonyl tungsten, hexacarbonyl molybdenum, and ethyl alcohol. The morphology and phase of the prepared products were highly dependent on the synthesis conditions such as synthesis and annealing temperature, synthesis time, and precursor ratio. The tungsten oxide nanostructures (TCNs) have urchin-like or spherical nanostructure with different phase of W18O49 and WO3. The morphology of tungsten-molybdenum oxide nanostructures (TMONs) is basically similar to that of TCNs. However, the morphology and phase of TMONs are more diverse and are strongly dependent on the composition ratios of W/Mo in the precursor. The electrochemical properties depending on their morphologies and phases of TCNs and TMONs are compared using cyclic voltammetry and galvanostatic charge/discharge tests. The relationship between the electrochromic performance and phase structures/morphologies of nanostructured TCNs and TMONs are systematically investigated.

Keywords: electrochemical, electrochromic, tungsten oxide, tungsten-molybdenum oxide

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Authors: B. M. Patil, S. R. Dharwadkar

Abstract:

Zirconolite (CaZrTi2O7) is one of the three major phases in the synthetic ceramic 'SYNROC' which is used for immobilization of high-level nuclear waste and also acts as photocatalytic and photophysical properties. In the present work the nanocrystalline CaZrTi2O7 was synthesized from Calcium Zirconyl Titanate tartrate precursor (CZTT) employing two different heating techniques such as Conventional heating (Muffle furnace) and Microwave heating (Microwave Oven). Thermal decomposition of the CZTT precursors in air yielded nanocrystalline CaZrTi2O7 powder as the end product. The products obtained by annealing the CZTT precursor using both heating method were characterized using simultaneous TG-DTA, FTIR, XRD, SEM, TEM, NTA and thermodilatometric study. The physical characteristics such as crystallinity, morphology and particle size of the product obtained by heating the CZTT precursor at the different temperatures in a Muffle furnace and Microwave oven were found to be significantly different. The microwave heating technique considerably lowered the synthesis temperature of CaZrTi2O7. The influence of microwave heating was more pronounced as compared to Muffle furnace heating. The details of the synthesis of CaZrTi2O7 from CZTT precursor are discussed.

Keywords: CZTT, CaZrTi2O7, microwave, SYNROC, zirconolite

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Authors: Omar Drissi, Nadia El Harfaoui, Khalid Nouneh, Rachid Hsissou, Badre Daoudi

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The pulp endures of having a lower importance, incompletely because of the way that it has been less studied, and it has been recognized as a pivotal product got from biomass that can be utilized in different fields. The current research focuses on pulp of Argania spinosa (L). To this end, the aim is to study the characteristics and properties of Argan pulp, such as shape, chemical and macromineral composition. As a result, X-Ray Fluorescence (XRF), Fourier transform infrared spectroscopy (FTIR), and Scanning Electron Microscopy (SEM) were used in the research.

Keywords: argania spinose, argan pulp, argan bio-waste, green synthesis, silver nanoparticles, valorization

Procedia PDF Downloads 122

Authors: Kumar N., Verma S., Park J., Srivastava V. C.

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Organic carbonates have the potential to be used as fuels and because of this, their production through non-phosgene routes is a thrust area of research. Di-ethyl carbonate (DEC) synthesis from propylene carbonate (PC) in the presence of alcohol is a green route. In this study, the use of reduced graphene oxide (rGO) based metal oxide catalysts [rGO-MO, where M = Ce] with different amounts of graphene oxide (0.2%, 0.5%, 1%, and 2%) has been investigated for the synthesis of DEC by using PC and ethanol as reactants. The GO sheets were synthesized by an electrochemical process and the catalysts were synthesized using an in-situ method. A theoretical study of the thermodynamics of the reaction was done, which revealed that the reaction is mildly endothermic. The theoretical value of optimum temperature was found to be 420 K. The synthesized catalysts were characterized for their morphological, structural and textural properties using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), N2 adsorption/desorption, thermogravimetric analysis (TGA), and Raman spectroscopy. Optimization studies were carried out to study the effect of different reaction conditions like temperature (140 °C to 180 °C) and catalyst dosage (0.102 g to 0.255 g) on the yield of DEC. Amongst the various synthesized catalysts, 1% rGO-CeO2 gave the maximum yield of DEC.

Keywords: GO, DEC, propylene carbonate, transesterification, thermodynamics

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Authors: Juree Hong, Sanggeun Lee, Jungmok Seo, Taeyoon Lee

Abstract:

We report a facile synthesis of metal nano particles (NPs) on graphene layer via galvanic displacement reaction between graphene-buffered copper (Cu) and metal ion-containing salts. Diverse metal NPs can be formed on graphene surface and their morphologies can be tailored by controlling the concentration of metal ion-containing salt and immersion time. The obtained metal NP-decorated single-layer graphene (SLG) has been used as hydrogen gas (H2) sensing material and exhibited highly sensitive response upon exposure to 2% of H2.

Keywords: metal nanoparticle, galvanic displacement reaction, graphene, hydrogen sensor

Procedia PDF Downloads 427

Authors: Delele Worku Ayele, Bing-Joe Hwang

Abstract:

A method that does not employ hot injection techniques has been developed for the size-tunable synthesis of high-quality CdSe quantum dots (QDs) with a zinc blende structure. In this environmentally benign synthetic route, which uses relatively less toxic precursors, solvents, and capping ligands, CdSe QDs that absorb visible light are obtained. The size of the as-prepared CdSe QDs and, thus, their optical properties can be manipulated by changing the microwave reaction conditions. The QDs are characterized by XRD, TEM, UV-vis, FTIR, time-resolved fluorescence spectroscopy, and fluorescence spectrophotometry. In this approach, the reaction is conducted in open air and at a much lower temperature than in hot injection techniques. The use of microwaves in this process allows for a highly reproducible and effective synthesis protocol that is fully adaptable for mass production and can be easily employed to synthesize a variety of semiconductor QDs with the desired properties. The possible application of the as-prepared CdSe QDs has been also assessed using deposition on TiO2 films.

Keywords: CdSe QDs, Na2SeSO3, microwave (MW), oleic acid, mass production, average life time

Procedia PDF Downloads 710

Authors: Hanaa M. Abdelgawad, Mona Safar, Ayman M. Wahba

Abstract:

Real-time image and video processing is a demand in many computer vision applications, e.g. video surveillance, traffic management and medical imaging. The processing of those video applications requires high computational power. Therefore, the optimal solution is the collaboration of CPU and hardware accelerators. In this paper, a Canny edge detection hardware accelerator is proposed. Canny edge detection is one of the common blocks in the pre-processing phase of image and video processing pipeline. Our presented approach targets offloading the Canny edge detection algorithm from processing system (PS) to programmable logic (PL) taking the advantage of High Level Synthesis (HLS) tool flow to accelerate the implementation on Zynq platform. The resulting implementation enables up to a 100x performance improvement through hardware acceleration. The CPU utilization drops down and the frame rate jumps to 60 fps of 1080p full HD input video stream.

Keywords: high level synthesis, canny edge detection, hardware accelerators, computer vision

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Authors: Javiera Poblete, Fernando Gajardo, Katherina Fernandez

Abstract:

Graphene, and its derivatives such as graphene oxide (GO), are emerging nanoscopic materials, with interesting physical and chemical properties. From them, it is possible to develop three-dimensional macrostructures, such as aerogels, which are characterized by a low density, high porosity, and large surface area, having a promising structure for the development of materials. The use of GO as a precursor of these structures provides a wide variety of materials, which can be developed as a result of the functionalization of their oxygenated groups, with specific compounds such as polyethylene glycol (PEG). The synthesis of aerogels of GO-PEG for non-covalent interactions has not yet been widely reported, being of interest due to its feasible escalation and economic viability. Thus, this work aims to develop a non-covalently functionalized GO-PEG aerogels and characterize them physicochemically. In order to get this, the GO was synthesized from the modified hummers method and it was functionalized with the PEG by polymer-assisted GO gelation (crosslinker). The gelation was obtained for GO solutions (10 mg/mL) with the incorporation of PEG in different proportions by weight. The hydrogel resulting from the reaction was subsequently lyophilized, to obtain the respective aerogel. The material obtained was chemically characterized by analysis of Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray diffraction (XRD), and its morphology by scanning electron microscopy (SEM) images; as well as water absorption tests. The results obtained showed the formation of a non-covalent aerogel (FTIR), whose structure was highly porous (SEM) and with a water absorption values greater than 50% g/g. Thus, a methodology of synthesis for GO-PEG was developed and validated.

Keywords: aerogel, graphene oxide, polyethylene glycol, synthesis

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Authors: Elmeliani M’Hammed

Abstract:

The work is carried out for the synthesis of antifungal effective against the fungus Fusarium oxysporum, Albedinis (Foa), the causative agent of bayoud, dates palm disease, through the use of raw clay as a green catalyst. The Aza-Michael reaction of amine addition to α, β-unsaturated alkene was carried out using the crude clay as a green catalyst to synthesize the antifungal agent bayoud. The reaction was carried out under favorable conditions, ambient temperature, without solvent, and a green catalyst "loves the environment" that the product that was synthesized gave us a high yield and excellent chemo selectivity.

Keywords: raw clay, amines, alkenes, environment, antifungal, bayoud, date palms

Procedia PDF Downloads 101

Authors: M. Yildirim, A. S. Kipcak, F. T. Senberber, M. O. Asensio, E. M. Derun, S. Piskin

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Potassium borates, which are widely used in welding and metal refining industry, as a lubricating oil additive, cement additive, fiberglass additive and insulation compound, are one of the important groups of borate minerals. In this study the production of a potassium borate mineral via hydrothermal method is aimed. The potassium source of potassium nitrate (KNO3) was used along with a sodium source of sodium hydroxide (NaOH) and boron source of boric acid (H3BO3). The constant parameters of reaction temperature and reaction time were determined as 80°C and 1 h, respectively. The molar ratios of 1:1:3 (as KNO3:NaOH:H3BO3), 1:1:4, 1:1:5, 1:1:6 and 1:1:7 were used. Following the synthesis the identifications of the produced products were conducted by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). The results of the experiments and analysis showed in the ratio of 1:1:6, the Santite mineral with powder diffraction file number (pdf no.) of 01-072-1688, which is known as potassium pentaborate (KB5O8•4H2O) was synthesized as best.

Keywords: hydrothermal synthesis, potassium borate, potassium nitrate, santite

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Authors: Ambika Selvaraj

Abstract:

Magnetic iron oxide nanoparticles (IO) of < 20nm (superparamagnetic) become promising tool in cancer therapy, and integrated nanodevices for cancer detection and screening. The obstacles include particle heterogeneity and cost. It can be overcome by developing monodispersed nanoparticles in economical approach. We have successfully synthesized < 7 nm IO by low temperature controlled technique, in which Fe0 is sandwiched between stabilizer and Fe2+. Size analysis showed the excellent size control from 31 nm at 33°C to 6.8 nm at 10°C. Resultant monodispersed IO were found to be stable for > 50 reuses, proved its applicability in biomedical applications.

Keywords: low temperature synthesis, hybrid iron nanoparticles, cancer therapy, biomedical applications

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Authors: Abdulkareem M. Hamid, Yaseen Elhebshi, Adam Daïch

Abstract:

Luotonins and its derivatives (Isoluotonins) are alkaloids from the aerial parts of Peganum nigellastrum Bunge that display three major skeleton types. Luotonins A, B, and E are pyrroloquinazolinoquinoline alkaloids. A few methods were known for the sysnthesis of Isoluotonin. All luotonins have shown promising cytotoxicities towards selected human cancer cell lines, especially against leukemia P-388 cells. Luotonin A is the most active one, with its activity stemming from topoisomerase I-dependent DNA-cleavage. Such intriguing biological activities and unique structures have led not only to the development of synthetic methods for the efficient synthesis of these compounds, but also to interest in structural modifications for improving the biological properties. Recent progress in the study of luotonins is covered.

Keywords: luotonin A, isoluotonin, pyrroloquiolines, alkaloids

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Authors: Dipali Nagaonkar, Mahendra Rai

Abstract:

Chitosan, a carbohydrate polymer at nanoscale level has gained considerable momentum in drug delivery applications due to its inherent biocompatibility and non-toxicity. However, conventional synthetic strategies for chitosan nanoparticles mainly rely upon physicochemical techniques, which often yield chitosan microparticles. Hence, there is an emergent need for development of controlled synthetic protocols for chitosan nanoparticles within the nanometer range. In this context, we report the green synthesis of size controlled chitosan nanoparticles by using Pongamia pinnata (L.) leaf extract. Nanoparticle tracking analysis confirmed formation of nanoparticles with mean particle size of 85 nm. The stability of chitosan nanoparticles was investigated by zetasizer analysis, which revealed positive surface charged nanoparticles with zeta potential 20.1 mV. The green synthesized chitosan nanoparticles were further explored for encapsulation and controlled release of antioxidant biomolecule, quercetin. The resulting drug loaded chitosan nanoparticles showed drug entrapment efficiency of 93.50% with drug-loading capacity of 42.44%. The cumulative in vitro drug release up to 15 hrs was achieved suggesting towards efficacy of green synthesized chitosan nanoparticles for drug delivery applications.

Keywords: Chitosan nanoparticles, green synthesis, Pongamia pinnata, quercetin

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Authors: Gülşah Çelik Gül, Figen Kurtuluş

Abstract:

Cesium molybdates with general formula CsMIII(MoO4)2, where MIII = Bi, Dy, Pr, Er, exhibit rich polymorphism, and crystallize in a layered structure. These properties cause intensive studies on cesium molybdates. CsBi(MoO4)2 was synthesized by microwave method by using cerium sulphate, bismuth oxide and molybdenum (VI) oxide in an appropriate molar ratio. Characterizations were done by x-ray diffraction (XRD), fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS), thermo gravimetric/differantial thermal analysis (TG/DTA).

Keywords: cesium bismuth dimolybdate, microwave synthesis, powder x-ray diffraction, rare earth dimolybdates

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Authors: Poonam Malik, Ravi Bhushan

Abstract:

This work describes a very efficient approach for synthesis of activated ester of (S)-naproxen which was characterized by UV, IR, ¹HNMR, elemental analysis and polarimetric studies. It was used as a C-N bond forming chiral derivatizing reagent for further synthesis of diastereomeric amides of (RS)-salbutamol (a β₂ agonist that belongs to the group β-adrenolytic and is marketed as racamate) under microwave irradiation. The diastereomeric pair was separated by achiral phase HPLC, using mobile phase in gradient mode containing methanol and aqueous triethylaminephosphate (TEAP); separation conditions were optimized with respect to pH, flow rate, and buffer concentration and the method of separation was validated as per International Council for Harmonisation (ICH) guidelines. The reagent proved to be very effective for on-line sensitive detection of the diastereomers with very low limit of detection (LOD) values of 0.69 and 0.57 ng mL⁻¹ for diastereomeric derivatives of (S)- and (R)-salbutamol, respectively. The retention times were greatly reduced (2.7 min) with less consumption of organic solvents and large (α) as compared to literature reports. Besides, the diastereomeric derivatives were separated and isolated by preparative HPLC; these were characterized and were used as standard reference samples for recording ¹HNMR and IR spectra for determining absolute configuration and elution order; it ensured the success of diastereomeric synthesis and established the reliability of enantioseparation and eliminated the requirement of pure enantiomer of the analyte which is generally not available. The newly developed reagent can suitably be applied to several other amino group containing compounds either from organic syntheses or pharmaceutical industries because the presence of (S)-Npx as a strong chromophore would allow sensitive detection.This work is significant not only in the area of enantioseparation and determination of absolute configuration of diastereomeric derivatives but also in the area of developing new chiral derivatizing reagents (CDRs).

Keywords: chiral derivatizing reagent, naproxen, salbutamol, synthesis

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Authors: Cecilia Espindola, Juan Carlos Palacios

Abstract:

Flavonoids are a large group of natural compounds which are found in many fruits and vegetables. A subgroup of these called flavanones display a wide range of biological activities, and they also have an important physiological role in plants. The ionic liquid (ILs) are compounds consisting of an organic cation with an organic or inorganic anion. Due to its unique properties such as high electrical conductivity, wide temperature range of the liquid state, thermal and electrochemical stability, high ionic density and low volatility and flammability, are considered as ecological solvents in organic synthesis, catalysis, electrolytes in accumulators, and electrochemistry, non-volatile plasticizers, and chemical separation. It was synthesized ionic liquid IL 1-butyl-3-methylimidazolium bromide free-solvent and used as reaction medium for flavanones synthesis, under several reaction conditions of temperature, time and production. The obtained compounds were analyzed by melting point, elemental analysis, IR and UV-vis spectroscopy.

Keywords: 1-butyl-3-methylimidazolium bromide, flavonoids, free-solvent, IR spectroscopy

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Authors: Samadhan S. Nagane, Sachin S. Kuhire, Prakash P. Wadgaonkar

Abstract:

Lignocellulose-derived chemicals such as furfural, furandicarboxylic acid, syringol, guaiacol, etc are highly attractive as sustainable alternatives to petrochemicals for the synthesis of monomers and polymers. We wish to report herein the facile synthesis of fully bio-based bisphenols containing pendant furyl group by base-catalyzed condensation of furfural with guaiacol. Bisphenols possessing pendant furyl group represent valuable monomers for the synthesis of a range of polymers which include epoxy resins, polyesters, polycarbonates, poly(aryl ether)s, etc. Several new homo/co-poly(arylene ether sulfone)s have been prepared by the reaction of 4,4(-fluorodiphenyl sulfone (FDS) with 4,4'-(furan-2-ylmethylene)bis(2-methoxyphenol) (BPF) and 4,4(-isopropylidenediphenol (BPA) using different molar ratios of bisphenols. Poly(arylene ether sulfone)s showed inherent viscosities in the range 0.92-1.47 dLg-1 and number average molecular weights (Mn), obtained from gel permeation chromatography (GPC), were in the range 91,300 – 1,31,000. Poly(arylene ether sulfone)s could be cast into tough, transparent and flexible films from chloroform solutions. X-Ray diffraction studies indicated amorphous nature of poly(arylene ether sulfone)s. Poly(arylene ether sulfone)s showed Tg values in the range 179-191 oC. Additionally, the pendant furyl groups in poly(arylene ether sulfone)s provide reactive sites for chemical modifications and cross-linking via Diels-Alder reaction with maleimides and bismaleimides, respectively.

Keywords: bio-based, bisphenols, Diels-Alder reaction, poly(arylene ether sulfone)s

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Authors: Sara Torabi, Sadegh Khazalpour, Mahdi Jamshidi

Abstract:

Nitro aromatic compounds are valuable materials because of their applications in the preparation of chemical intermediates for the synthesis of dyes, plastics, perfumes, energetic materials, and pharmaceuticals. Chemical and electrochemical procedures are reported for nitration of aromatic compounds. Flavonoid derivatives are present in many vegetables and fruits and are constituent of many common pharmaceuticals and dietary supplements. Electrochemistry provides very versatile means for the electrosynthesis, mechanistic and kinetic studies. To the best of our knowledge, and despite the importance of these compounds in numerous scientific fields, there are no reports on the electrochemical nitration of Quercetin derivatives. Herein, we describe a green electrochemical synthesis of a nitro compound. In this work, electrochemical oxidation of Quercetin has been studied in the presence of nitrite ion as a nucleophile in acetate buffer solution (c = 0.2 M, pH = 6.0), by means of cyclic voltammetry and controlled-potential coulometry. The results indicate the participation of produced o-benzoquinones in Michael reaction with nitrite ion (in the divided cell) to form the corresponding nitro diol (EC mechanism). The purity of product and characterization was done using ¹H NMR, ¹³C NMR, FTIR spectroscopic techniques. The presented strategies use a water/ethanol mixture as solvent. Ethanol as cosolvent was also used in the previous studies because of its low cost, safety, easy availability, recyclability, bioproductability, and biodegradability. These strategies represent a one-pot and facile process for the synthesis of nitro compound in high yield and purity under green conditions.

Keywords: electrochemical synthesis, green chemistry, cyclic voltammetry, molecular docking

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Authors: A. Belmokhtar, A. Yahiaoui, A. Benyoucef, M. Belbachir

Abstract:

We reported the synthesis and characterization of nanocomposite poly (4,4’ methylenedianiline) via chemical polymerization of monomers 4,4’ methylenedianiline by ammonium persulfate (APS) at room temperature catalyzed by Maghnite-H+. A facile method was demonstrated to grow poly (4,4’ methylenedianiline) nanocomposite, which was carried out by mixing Ammonium Persulfate (APS) aqueous and 4,4’ methylenedianiline solution in the presence of Maghnite-H+ at room temperature The effect of amount of catalyst and time on the polymerization yield of the polymers was studied. Structure was confirmed by elemental analysis, UV vis, RMN-1H, and voltammetry cyclique.

Keywords: charaterization, maghnite-h+, polymerization, poly (4, 4’ methylenedianiline)

Procedia PDF Downloads 289

Authors: M. Vijaya Bhaskar Reddy

Abstract:

The air-dried and powdered methanol solvent extraction of the rhizomes of Alpinia galangal is subjected to bio-assay guided fractionation and isolation yielded a known compound namely, 1'-S-1'-Acetoxychavicol acetate (1). The isolated known compound has been identified based on the physical, spectral data (IR, ¹H, ¹³C, NMR and mass spectroscopy) and comparison with an authentic sample. Finally isolated 1'-S-1'-Acetoxychavicol acetate (1) was confirmed by synthesis. The crude methanol extract and identified known compound (1) were tested for antidandruff property against Malassezia furfur showed with MIC 1000 µg/mL and 7.81 µg/mL, respectively.

Keywords: Alpinia galanga, isolation, 1'-S-1'-Acetoxychavicol acetate, antidandruff activity, Malassezia furfur

Procedia PDF Downloads 172

Authors: Hong Su, Qiuju Yan, Wei Du, En Hu, Zhaoyu Yang, Wei Zhang, Yusheng Li, Tao Tang, Wang yang, Shushan Zhao

Abstract:

Osteoarthritis (OA) is a severe chronic inflammatory disease. As the main active component of Astragalus mongholicus Bunge, a classic traditional ethnic herb, calycosin exhibits anti-inflammatory action and its mechanism of exact targets for OA have yet to be determined. In this study, we established an anterior cruciate ligament transection (ACLT) mouse model. Mice were randomized to sham, OA, and calycosin groups. Cartilage synthesis markers type II collagen (Col-2) and SRY-Box Transcription Factor 9 (Sox-9) increased significantly after calycosin gavage. While cartilage matrix degradation index cyclooxygenase-2 (COX-2), phosphor-epidermal growth factor receptor (p-EGFR), and matrix metalloproteinase-9 (MMP9) expression were decreased. With the help of network pharmacology and molecular docking, these results were confirmed in chondrocyte ATDC5 cells. Our results indicated that the calycosin treatment significantly improved cartilage damage, this was probably attributed to reversing the imbalance between chondrocyte synthesis and catabolism.

Keywords: calycosin, osteoarthritis, network pharmacology, molecular docking, inflammatory, cyclooxygenase 2

Procedia PDF Downloads 106

Authors: Cheng Shen, LaiHong Shen

Abstract:

Ammonia is an important carrier of hydrogen energy, with the characteristics of high hydrogen content density and no carbon dioxide emission. Ammonia synthesis by the Haber process is the main method for industrial ammonia synthesis, but the conversion rate of ammonia per pass is only about 12%, while the conversion rate of biomass synthesis ammonia is as high as 56%. Therefore, safe and efficient ammonia capture for ammonia synthesis from biomass is an important way to alleviate the energy crisis and solve the energy problem. Metal chloride has a chemical adsorption effect on ammonia, and can be desorbed at high temperature to obtain high-concentration ammonia after combining with ammonia, which has a good development prospect in ammonia capture and separation technology. In this paper, the ammonia adsorption properties of CuCl₂ were measured, and the composite adsorbents were prepared by using silicon and multi-walled carbon nanotubes respectively to support CuCl₂, and the ammonia adsorption properties of the composite adsorbents were studied. The study found that the ammonia adsorption capacity of the three adsorbents decreased with the increase in temperature, so metal chlorides were more suitable for the low-temperature adsorption of ammonia. Silicon and multi-walled carbon nanotubes have an enhanced effect on the ammonia adsorption of CuCl₂. The reason is that the porous material itself has a physical adsorption effect on ammonia, and silicon can play the role of skeleton support in cupric chloride particles, which enhances the pore structure of the adsorbent, thereby alleviating sintering.

Keywords: ammonia, adsorption properties, metal chloride, silicon, MWCNTs

Procedia PDF Downloads 113