122 research outputs found
Preconcentration of Co, Ni, Cd and Zn on naphthalene–2,4,6-trimorpholino-1,3,5-triazin adsorbent and flame atomic absorption determination
A preconcentration method was developed for the determination of trace amounts of Co, Ni, Cd and Zn by atomic absorption spectrometry. The method is based on the retention of the metal cations by naphthalene–2,4,6-trimorpholino-1,3,5-triazin adsorbent in a column. The adsorbed metals were then eluted from the column with hydrochloric acid and the Co, Ni, Cd and Zn were determined by flame atomic absorption spectrometry. The optimal extraction and elution conditions were studied. The effects of diverse ions on the preconcentration were also investigated. A preconcentration factor of 250 for Co(II), Ni(II) and Zn(II), and 400 for Cd(II) can easily be achieved. Calibration graphs were obtained and the detection limits of the method for Co(II), Ni(II), Cd(II) and Zn(II) were 0.51, 0.49, 0.17 and 0.10 ng mL-1, respectively. The relative standard deviations (RSD) of 0.37–2.31 % for Co, 0.37–3.73 % for Ni, 2.20–2.40 % for Cd and 1.50–2.56 % for Zn were obtained. The method was also used for the simultaneous preconcentration of these elements and the method was successfully applied to their preconcentration and determination. The method was applied to the determination of Co, Ni, Cd and Zn in several real samples
Molybdatophosphoric acid as an efficient catalyst for the catalytic and chemoselective oxidation of sulfides to sulfoxides using urea hydrogen peroxide as a commercially available oxidant
An efficient procedure for the chemoselective oxidation of alkyl (aryl) sulfides to the corresponding sulfoxides using urea hydrogen peroxide (UHP) in the presence of a catalytic amount of molybdatophosphoric acid at room temperature is described. The advantages of described method are: generality, high yield and chemoselectivity, short reaction time, low cost and compliment with green chemistry protocols
Synthesis of 1,4-Dihydropyridines Bearing a Carbamate Moiety on the 4-Position
A good range of 1,4-dihydropyridines bearing a carbamate moiety on the 4-position were synthesized from the primary reaction of different hydroxyaldehydes with phenyl isocyanates and the subsequent reaction of the obtained carbamates with methyl acetoacetate in the presence of ammonium fluoride. When phenyl isothiocyanate was used in place of phenyl isocyanate in the same condition, the reaction did not take place
Synthesis of Nano Magnetite Fe3O4 Based Vanadic Acid: A Highly Efficient and Recyclable Novel Nano-catalyst for the Synthesis of 4,4’-(arylmethylene)-bis(3-methyl-1-phenyl-1H-pyrazol-5-ols)
Nano magnetic Fe3O4 based vanadic acid [MNPs@VO(OH)2] (average diameter 20–26 nm) has been synthesized by grafting VOCl3 on the Fe3O4 surface nanoparticles as a retrievable supporter to produce novel heterogeneous reusable solid acid with dual ability (Bronsted and Lewis acid) followed by stirring in the air. The resultant material was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) analysis and energy-dispersive X-ray spectroscopy (EDX). Significantly, the as-prepared [MNPs@VO(OH)2] exhibits a high catalytic activity in the synthesis of 4,4’-(arylmethylene)bis(3-methyl-1-phenyl-1H-pyrazol-5-ols). Additionally, the newly synthesized heterogeneous solid acid catalyst can be reused for several times without apparent loss of its catalytic activity.
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Metal-free catalytic oxidation of sulfides to sulfoxides with ammonium nitrate, ammonium hydrogen sulfate and ammonium bromide as catalyst
A general and metal-free catalytic oxidation of aliphatic and aromatic sulfides to their corresponding sulfoxides via combination of ammonium nitrate (NH4NO3), supported ammonium hydrogen sulfate on silica gel (NH4HSO4-SiO2) and a catalytic amount of ammonium bromide (NH4Br) in the presence of wet SiO2 (50%, w/w) has been investigated. The reactions were carried out heterogeneously and selectively in short reaction times in CH2Cl2 at room temperature. This protocol is mild and efficient compared to other reported methods
One-pot three-component synthesis of 4,4-(arylmethylene)bis(3-methyl-1-phenyl-1H-pyrazol-5-ols) using silica vanadic acid as heterogeneous and recyclable catalyst with dual ability
Silica vanadic acid (oxo-vanadium has been supported on silica) with Lewis and Bronsted acid site is introduced as an efficient, reusable, and heterogeneous catalyst for tandem Knoevenagel–Michael reaction of two equivalents of 5-methyl-2-phenyl-2,4-dihydro-3H-pyrazol-3-one with various aromatic aldehydes for the synthesis of 4,4′-(arylmethylene)bis(1H-pyrazol-5-ol)s at room temperature. The present methodology offers several advantages over existing methodologies, such as excellent yields, short reaction time, simple procedure, easy work-up, mild reaction conditions, and synthesis of wide range of products. This procedure gave the products in excellent yields within very short reaction times over other vanadium(V) compounds. Also this catalyst can be reused six times without appreciable loss of its catalytic activity
Solvent-free Preparation of 1,1-Diacetates from Aldehydes Mediated by Zirconium Hydrogen Sulfate at Room Temperature
A mild and efficient method has been developed for the preparation of acylals in good yields through a reaction of aldehydes with acetic anhydride using Zr(HSO 4 ) 4 as catalyst at room temperature and under solvent-free conditions
Facile preparation of a nanostructured functionalized catalytically active organosalt
We report a novel nanostructured organosalt, based on sulfonic acid
functionalized pyrazinium {[H-pyrazine–SO3H]Cl2} that was synthesized and
characterized by several techniques including Fourier transform infrared (FT-
IR) spectroscopy, X-ray diffraction (XRD), thermal gravimetric analysis (TGA),
differential thermal gravimetric (DTG) analysis, transmission electron
microscopy (TEM), mass spectrometry (MS), proton NMR (1H NMR), carbon-13 NMR
(13C NMR) and also electron diffraction (ED) patterns. Results proved that the
unprecedented sulfonated pyrizinium organosalt is indeed nanostructured and
highly crystalline as supported by TEM, ED and XRD studies, having an average
nanoparticle size of 50 nm according to TEM micrographs. The novel nano-
organocatalyst was proved to be an efficient catalyst in the synthesis of
1,2,4,5-tetrasubstituted imidazoles by a one-pot multi-component condensation
of benzil, a broad range of aldehydes, primary amines and ammonium acetate at
90 °C under solvent-free conditions
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