Efficient synthesis of novel pyrazole-linked 1,2,4-triazolidine-3-thiones using bismuth on zirconium oxide as a recyclable catalyst in aqueous medium

Molecular Diversity - The Bi2O3 loading on ZrO2 as heterogeneous catalyst was established as an extremely efficient catalyst for the synthesis of a series of novel...     

Efficient and green synthesis of tetrasubstituted pyrroles promoted by task-specific basic ionic liquids as catalyst in aqueous media

Synthesis of tetrasubstituted pyrroles by the three-component condensation reaction of acid chlorides, dialkyl acetylenedicarboxylates, and amino acids in the presence of various room-temperature ionic liquids (RTILs) as catalysts in water is reported. Among the ionic liquids used, the basic functionalized ionic liquid, butyl methyl imidazolium hydroxide [bmim]OH, was the most effective catalyst. The influence of reaction temperature, reaction time, and amount of ionic liquid on the reaction was investigated. The [bmim]OH/H₂O catalyst system could be reused for at least five recycles without appreciable loss of efficiency.     

Sonochemical activation in aqueous medium for solid-state synthesis of BaTiO3 powders

BaTiO₃-based oxide compounds are important ceramic materials for multilayer ceramic capacitors. In this paper, we report a sonochemical activation process of BaCO₃ and TiO₂ in an aqueous medium for the synthesis of BaTiO₃ powders through a solid-state process. Owing to the physical and chemical effects of the ultrasonication in aqueous medium on the raw materials, BaTiO₃ powders could be successfully synthesized at relatively low temperatures through a solid-state reaction, which was significantly enhanced as compared to the case in ethanol medium. Detailed investigations on the resulting BaTiO₃ powders and ceramics were performed, and a model to understand the role of aqueous medium on the enhancement of the solid-state reaction was proposed in terms of Ba²⁺ ion leaching and zeta potential of TiO₂, which are strongly affected by the pH of the aqueous medium. Our results are not only helpful for cost-effective synthesis of BaTiO₃ through the highly reliable solid-state reaction process, but they also provide an understanding of the role of aqueous medium for the sonochemical process using raw materials with partial solubility in water.     

An environment-friendly methodology for the construction of diversified bicycloacenaphtho[1,2-d]imidazole-8-thione scaffolds using spinel NiFe2O4 nanoparticles as a sustainable catalyst

Molecular Diversity - Herein, we successfully developed an easy access to bicycloacenaphtho[1,2-d]imidazole-8-thione by one-pot three-component MCRs of acenaphthoquinone, aryl or alkyl...     

Sulfonated magnetic sugarcane bagasse as an efficient natural polymer-based catalyst for the synthesis of nitrogen-containing heterocyclic rings in water

Molecular Diversity - A new species of catalysts that are prepared from biocompatible materials is demonstrated. Sulfonated magnetic sugarcane bagasse has been synthesized as a novel biodegradable...     

Water extract of red mud: an efficient and renewable medium for environmentally benign synthesis of 2-amino-4H-chromenes

Molecular Diversity - In this study, an efficient and convenient domino Michael addition/intramolecular cyclization protocol is presented for the synthesis of biologically relevant...     

A one-pot synthesis of piperidinium spirooxindoline-pyridineolates and indole-substituted pyridones in aqueous or ethanol medium

Molecular Diversity - Piperidinium spirooxindoline-pyridineolate has been prepared via one-pot multicomponent reaction of isatin, malononitrile, cyanoacetohydrazide, and piperidine in water or...     

A simple and rapid protocol for the synthesis of phenacyl derivatives using macroporous polymer-supported reagents

This article describes the use of Amberlite IRA-910 with different counter ions as excellent polymer-supported reagents in nucleophilic substitution reactions. The versatility of this protocol allowed the synthesis of a diversified library of phenacyl derivatives with high yields. The polymeric reagents can be reloaded several times with no loss of their efficiency.     

Microwave assisted one pot synthesis of biocompatible gold nanoparticles in Triton X-100 aqueous micellar medium using tryptophan as reducing agent

The present work reports an environmentally benign process for the synthesis of gold nanoparticles via microwave-assisted heating method, using a basic amino acid l-Tryptophan as reducing agent. The synthesis was carried out in the presence of a nonionic surfactant Triton X-100 (TX-100) aqueous micellar system. Influence of various reaction parameters such as microwave irradiation time and concentrations of precursor ion were analyzed. The effect of pH on the plasmonic properties and stability of synthesized AuNPs were studied in detail. The various size distributions of gold nanostructures obtained were characterized and analyzed by ultraviolet visible spectroscopy (UV-Vis), TEM and DLS analysis. Fourier transform infrared (FT-IR) measurements were carried out to identify the interaction sites responsible for capping and efficient stabilization by the amino acid as well as the surfactant. The synthesized gold nanoparticles were stable for more than 6 months at ambient conditions.     

Improved direct synthesis of TiO2 catalyst using sonication and its application for the desulfurization of thiophene

TiO₂ catalyst was synthesized in the presence of ultrasound (ultrasonic horn at 20 kHz frequency and 70% duty cycle) at different power (80 W to 120 W) and durations as well as surfactant concentration with an objective of establishing best conditions for achieving lowest particle size of the photocatalyst. Detailed characterization in terms of crystal phase, crystallinity, functional groups and morphology of the photocatalyst has been performed using SEM, XRD and FTIR analysis. It was demonstrated that sonication significantly reduced the particle size with high degree of sphericity and homogeneity as compared to conventionally synthesized TiO₂ with similar crystallinity in both cases. The catalytic performance was subsequently evaluated for the deep desulfurization of thiophene. Different desulfurization approaches including individual US (ultrasonic horn at 20 kHz frequency, 110 W power and 70% duty cycle) and UV irradiations, US/UV, US/UV/H₂O₂, US/UV/TiO₂ and US/UV/H₂O₂/TiO₂ were applied to evaluate the catalytic activity. The best approach was demonstrated as US/UV/H₂O₂/TiO₂ and also activity of catalyst synthesized using ultrasound was much better compared to conventionally synthesized catalyst. The studies related to different model solvents demonstrated lowest reactivity for toluene whereas n-hexane and n-octane resulted in complete desulfurization in 60 min and 50 min treatment respectively. The desulfurization followed pseudo first order reaction kinetics irrespective of the solvent used. Overall the work clearly demonstrated the efficacy of ultrasound in improving the catalyst synthesis as well as desulfurization of thiophene.     

Very rapid synthesis of highly efficient and biocompatible Ag2Se QD phytocatalysts using ultrasonic irradiation for aqueous/sustainable reduction of toxic nitroarenes to anilines with excellent yield/selectivity at room temperature

There are many problems associated with the synthesis of nanocatalysts and catalytic reduction of nitroarenes - e.g., high temperatures, costs, long reaction/synthesis process times, the toxicity of chemicals/solvents, undesirable byproducts, the toxic/harmful wastes, low efficiency/selectivity, etc. This study represents an attempt to overcome these challenges. To this purpose, biocompatible and highly efficient Ag₂Se quantum dots (QDs) catalysts with antibacterial activity were synthesized in a very rapid (30 sec, rt), simple, inexpensive, sustainable/green, and one-pot strategy in water using ultrasonic irradiation. Characterization of the QDs was performed using different techniques. UV–Vis absorption and fluorescence spectroscopic studies showed an absorption peak at 480–550 nm and a maximum emission peak around 675 nm, which confirmed the successful synthesis of Ag₂Se QDs via the applied biosynthetic method. Subsequently, catalytic reduction of nitroarenes by them was carried out under safe conditions (H₂O, rt, air atmosphere) in ∼ 60 min with excellent yield and selectivity (>99%). Their catalytic activity in the reduction of various toxic nitroarenes to aminoarenes under green conditions was investigated. Thus, a rapid and safe ultrasound-based method was employed to prepare stable and green Ag₂Se QDs phyto-catalysts with unique properties, including exquisite monodispersity in shape (orthorhombic) and size (∼7 nm), air-stability, and good purity and crystallinity. Importantly, instead of various toxic chemicals, the plant extract obtained by rapid ultrasonic method (10 min, rt) was used as natural reducing, capping, and stabilizing agents. Moreover, antibacterial assays results showed that Ag₂Se-QDs catalysts at low concentrations (ppm) have high activity against all tested bacteria, especially E. coli (MIC:31.25 ppm, MBC:125 ppm) which were significantly different from those of Fig extract (MIC = MBC:500 ppm). The data reflect the role of these bio-synthesized Ag₂Se-QDs catalysts in the development of versatile and very safe catalysts with biomedical properties.     

An efficient protocol for the synthesis of 2-amino-4,6-diphenylpyridine-3-carbonitrile using ionic liquid ethylammonium nitrate

Chalcones on condensation with malononitrile and ammonium acetate in the presence of ionic liquid ethylammonium nitrate affords the corresponding 2-amino-4, 6-diphenylpyridine-3-carbonitrile in excellent yield. The ionic liquid is recycled and reused several times.     

KSF: an efficient catalyst for the regioselective synthesis of 1,5-diaryl pyrazoles using Baylis–Hillman adducts

A facile and convenient protocol was developed for the regioselective synthesis of 1,5-diarylpyrazoles using Baylis–Hillman adducts over KSF catalyst in high yields (70–90%) and low reaction times.     

Ultrasound-promoted green approach for the synthesis of sulfonamides using natural,stable and reusable Natrolite nanozeolite catalyst at room temperature

Natural Natrolite nanozeolite has been investigated as an efficient and reusable catalyst for the N-sulfonylation of amines under ultrasound irradiation at room temperature. Compared with traditional methods, the significant advantages for method are green solvent, milder and cleaner conditions, higher purity and yields, shorter reaction time, easier work-up procedure and the lower generation of waste or pollutions. The catalyst can be recovered and reused several times without significant loss of its catalytic activity.     

A facile and environmentally friendly chemical route for the synthesis of metastable VO2 nanobelts

Metastable VO₂ nanobelts, designated as VO₂ (B), were successfully fabricated by a facile hydrothermal route in the presence of V₂O₅ and glucose. The samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), transmission electron microscopy (TEM), selected area electronic diffraction (SAED), high-resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM) techniques. The main synthesis parameters such as temperature, reaction time and molar ratio of the starting materials have been also discussed. The results showed that pure B phase VO₂ nanobelts with high crystallinity can be prepared easily at 180 °C in 24 h at the molar ratio of V₂O₅:glucose=1:1. Typically, the belt-like products were 0.6-1.2 μm long, 80-150 nm wide and 20-30 nm thick. It is noted that the whole process is free of any harmful reducing reagents and surfactants, and valuable gluconic acid can be formed as the main by-product. From an economic and environmental point of view, the present approach is particularly fit for the synthesis of VO₂ (B) nanobelts on a large scale.     

A novel continuous process for synthesis of carbon nanotubes using iron floating catalyst and MgO particles for CVD of methane in a fluidized bed reactor

A novel continuous process is used for production of carbon nanotubes (CNTs) by catalytic chemical vapor deposition (CVD) of methane on iron floating catalyst in situ deposited on MgO in a fluidized bed reactor. In the hot zone of the reactor, sublimed ferrocene vapors were contacted with MgO powder fluidized by methane feed to produce Fe/MgO catalyst in situ. An annular tube was used to enhance the ferrocene and MgO contacting efficiency. Multi-wall as well as single-wall CNTs was grown on the Fe/MgO catalyst while falling down the reactor. The CNTs were continuously collected at the bottom of the reactor, only when MgO powder was used. The annular tube enhanced the contacting efficiency and improved both the quality and quantity of CNTs.The SEM and TEM micrographs of the products reveal that the CNTs are mostly entangled bundles with diameters of about 10-20 nm. Raman spectra show that the CNTs have low amount of amorphous/defected carbon with I_G/I_D ratios as high as 10.2 for synthesis at 900 °C. The RBM Raman peaks indicate formation of single-walled carbon nanotubes (SWNTs) of 1.0-1.2 nm diameter.