One-pot synthesis of 2-amino-3-cyanopyridines and hexahydroquinolines using eggshell-based nano-magnetic solid acid catalyst via anomeric-based oxidation

Research on Chemical Intermediates - In the present research, the eggshell as a hazardous waste by European Union regulations was converted to a valuable catalyst, namely nano-Fe3O4@(HSO4)2. The...     

Aqueous media preparation of 2-amino-4,6-diphenylnicotinonitriles using cellulose sulfuric acid as an efficient catalyst

A convenient approach to the synthesis of 2-amino-4,6-diphenylnicotinonitriles via four-component reaction of aromatic aldehydes, acetophenone derivatives, malononitrile and ammonium acetate is described. The reactions were done in water as solvent using cellulose sulfuric acid as catalyst. This simple protocol offer advantages such as shorter reaction times, simple work-up procedure, excellent yields and catalyst recovery.     

Synthesis of a novel acidic ionic liquid catalyst and its application for preparation of pyridines via a cooperative vinylogous anomeric-based oxidation

Research on Chemical Intermediates - In the current study, a novel acidic ionic liquid catalyst based on 8-hydroxyquinoline, namely...     

Synthesis of magnetic CuFe2O4 nanoparticles as green catalyst for toluene oxidation under solvent-free conditions

A green method was developed for the synthesis of CuFe₂O₄ magnetic nanoparticles using a Neem leave extract. The prepared nanoparticles with an average size of 19.7 nm were used as an effective catalyst for the oxidation of various aryl alkanes in moderate to excellent yields under solvent-free conditions. The catalyst was characterized by powder- XRD, SEM and TEM study. The key advantages of this protocol are simple preparation, a recyclable heterogeneous catalytic system, and benign reaction condition with good to excellent yields with high selectivity toward acid (42–87%).     

PbS nanoparticles stabilized on HPG-modified FeNi3 as catalyst for synthesis of 2-amino-4H-chromene under mild conditions

FeNi₃\SiO₂\HPG\PbS magnetic nanoparticles (MNPs) catalyst was readily prepared from inexpensive starting materials in aqueous media which catalyzed the synthesis 2-amino-4H-chromene via intermittent microwave irradiation. X-ray diffraction, transmission electron micrographs, and scanning electron micrographs were employed to characterize the properties of the synthesized FeNi₃\SiO₂\HPG\PbS MNPs. High catalytic activity and ease of recovery from the reaction mixture using external magnet and several reuse times without significant losses in performance are additional eco-friendly attributes of this catalytic system.     

Poly N,N-dimethylaniline-formaldehyde supported on silica-coated magnetic nanoparticles: a novel and retrievable catalyst for green synthesis of 2-amino-3-cyanopyridines

Research on Chemical Intermediates - Preparation and application of novel and reusable magnetic nanoparticles with poly N,N-dimethylaniline-formaldehyde support as a heterogeneous basic catalyst...     

A simple synthesis of magnetic nanoparticles-supported 4-aminomethylbenzoic acid as a highly efficient and reusable catalyst for synthesis of 2-amino-4H-chromene derivatives

Research on Chemical Intermediates - A new 4-aminomethylbenzoic acid-functionalized Fe3O4 magnetic nanoparticles as a hybrid heterogeneous catalyst was synthesised and characterized by FT-IR, XRD,...     

Nanosized magnesium oxide as catalyst for the rapid and green synthesis of substituted 2-amino-2-chromenes

A nanosized magnesium oxide catalyzed three-component condensation reaction of aldehyde, malononitrile, and α-naphthol proceeded rapidly in water-PEG to afford corresponding 2-amino-2-chromenes in high yields at room temperature. The greener protocol was found to be fairly general and the catalyst was reused in subsequent reactions with consistent activity.     

Synthesis of 2-amino-4,6-dimethoxypyrimidine with dimethyl carbonate as methylating agent

2-amino-4,6-dimethoxypyrimidine (ADM) was prepared from 2-amino-4,6-dihydroxypyrimidine (ADH) in the presence of potassium carbonate and phase transfer catalyst (PTC), with dimethyl carbonate (DMC) instead of conventional toxic reagents (such as haloalkane and dimethyl sulfate, etc.). The best conversion (87.7 %) of ADH and selectivity (40.5 %) toward ADM were achieved under optimized conditions: tetrabutyl ammonium bromide (TBAB) as PTC, n(ADH):n(DMC):n(TBAB):n(K₂CO₃) = 1:5:0.1:3, reaction time = 10 h and reaction temperature = 150 °C.     

Novel ferrocene-based ionic liquid supported on silica nanoparticles as efficient catalyst for synthesis of naphthopyran derivatives

We report synthesis of silica nanospheres containing ferrocene-tagged imidazolium acetate (SiO₂@Im-Fc[OAc]) as efficient heterogeneous nanocatalyst for synthesis of naphthopyran derivatives under solvent-free conditions, based on modification of nano SiO₂ by ionic liquid with ferrocene tags and subsequent anion metathesis reaction. The synthesized novel nanocatalyst (SiO₂@Im-Fc[OAc]) was systematically characterized using Fourier-transform infrared spectroscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction analysis, and field-emission scanning electron microscopy. The catalytic activity of (SiO₂@Im-Fc[OAc]) was tested in one-pot three-component reaction of aromatic aldehydes, malononitrile, and 2-naphthol for facile synthesis of naphthopyran derivatives. To achieve high catalytic efficacy, the effects of various reaction parameters such as temperature, amount of catalyst, type of solvent, etc. were investigated. Furthermore, recovery and reuse of the nanocatalyst several times was demonstrated without appreciable loss in catalytic activity. The presented protocol offers several advantages, including green and ecofriendly nature, operational simplicity, higher yield, and easy recovery and reuse of the nanostructured catalyst. The workup of these very clean reactions involves only recrystallization of the product from ethanol and recovery of the catalyst by filtration.     

Nitrogen-doped magnetic carbon nanoparticles as catalyst supports for efficient recovery and recycling

Palladium nanoparticles were deposited with high dispersion and stability on nitrogen-doped magnetic carbon nanoparticles by a simple impregnation method, and their catalytic performance was investigated for Heck, Suzuki, and Sonogashira coupling reactions.     

ZnO-nanorods as economical catalyst for synthesis of 4-amino-2-iminodithiole derivatives using tetramethyl thiourea in water

4-amino-2-iminodithiole derivatives were synthesised via multi-component reactions of tetramethyl thiourea, isothiocyanates and alkyl bromides in the presence of ZnO nanorods (ZnO-NR) as the catalyst in water at ambient temperature. These reactions provide low yields without catalysts. The catalyst exhibited significant reusable activity.     

Imidazole as an efficient catalyst for the synthesis of 2-amino-3-cyano-4H-chromen-4yl-phosphonates

An efficient procedure for the preparation of 2-amino-3-cyano-4H-chromen-4-yl phosphonate derivatives via a three-component reaction of salicylaldehyde, malononitrile and trialkyl phosphites or diethyl phosphite using inexpensive and environmentally friendly imidazole as organocatalyst has been reported. Beside excellent yields and easy workup, the reaction is done in an almost neutral medium.     

Detection of uranium with a wireless sensing method by using salophen as receptor and magnetic nanoparticles as signal-amplifying tags

A new wireless sensing method for the detection of uranium in water samples has been reported in this paper. The method is based on a sandwich-type detection strategy. Salophen, a tetradentate ligand of uranyl ion, was immobilized on the surface of the polyurethane-protected magnetoelastic sensor as receptor for the capture of uranyl ion. The phosphorylated polyvinyl alcohol coated magnetic Fe₃O₄ nanoparticles were used as signal-amplifying tags of uranyl ion. In a procedure of determining uranium, firstly uranyl ion in sample solution was captured on the sensor surface. Then the captured uranyl bound the nanoparticle through its coordination with the phosphate group. The amount of uranium was detected through the measure of the resonance frequency shift caused by the enhanced mass loading on the sensor surface. A linear range was found to be 0.2–20.0 μg/L under optimal conditions with a detection limit of 0.11 μg/L. The method has been applied to determine uranium in environmental water samples with the relative standard deviations of 2.1–3.6 % and the recoveries of 98.0–101.5 %. The present technique is one of the most suitable techniques for assay of uranium at trace level in environmental water samples collected from different sources.     

One‐pot synthesis of polysubstituted pyrrolidinones using novel magnetic nanoparticles as an efficient and reusable catalyst

7‐Aminonaphthalene‐1,3‐disulfonic acid‐functionalized magnetic Fe₃O₄ nanoparticles efficiently catalyse the one‐pot multi‐component synthesis of substituted 3‐pyrrolin‐2‐ones without using any other harmful organic reagents. High catalytic activity, ease of recovery, use of an external magnetic field and capability of being reused many times without significant loss of its catalytic activity are additional eco‐friendly properties of this catalytic system. Compared to other methods, our protocol has various advantages such as short reaction times, low catalyst loading, high yields, easy magnetic separation and reusability of the catalyst.     

Efficient anchorage of Pd nanoparticles on carbon nanotubes as a catalyst for hydrazine oxidation

A simple method is devised to deposit well-dispersed Pd nanoparticles on multi-walled carbon nanotubes (CNTs). Pd nanoparticles (1–3 nm) prepared in ethanol were transferred to toluene solution and modified by organic molecule benzyl mercaptan which acts as a cross linker between Pd nanoparticles and CNTs. The morphology and structure of the resulting Pd/CNT nanocomposite were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The results show that Pd nanoparticles were highly dispersed and effectively anchored on CNTs. The excellent electrocatalytic activity of the Pd/CNT nanocomposite for the oxidation of hydrazine was demonstrated by cyclic voltammetry.     

Ionic liquids as recycling solvents for the synthesis of magnetic nanoparticles

This work describes an easy synthesis (one pot) of MFe(2)O(4) (M = Co, Fe, Mn, and Ni) magnetic nanoparticles MNPs by the thermal decomposition of Fe(Acac)(3)/M(Acac)(2) by using BMI·NTf(2) (1-n-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide) or BMI·PF(6) (1-n-butyl-3-methylimidazolium hexafluorophosphate) ionic liquids (ILs) as recycling solvents and oleylamine as the reducing and surface modifier agent. The effects of reaction temperature and reaction time on the features of the magnetic nanomaterials (size and magnetic properties) were investigated. The growth of the MNPs is easily controlled in the IL by adjusting the reaction temperature and time, as inferred from Fe(3)O(4) MNPs obtained at 150 °C, 200 °C and 250 °C with mean diameters of 8, 10 and 15 nm, respectively. However, the thermal decomposition of Fe(Acac)(3) performed in a conventional high boiling point solvent (diphenyl ether, bp 259 °C), under a similar Fe to oleylamine molar ratio used in the IL synthesis, does not follow the same growth mechanism and rendered only smaller NPs of 5 nm mean diameter. All MNPs are covered by at least one monolayer of oleylamine making them readily dispersible in non-polar solvents. Besides the influence on the nanoparticles growth, which is important for the preparation of highly crystalline MNPs, the IL was easily recycled and has been used in at least 20 successive syntheses.