Palladium-catalyzed stereoselective synthesis of 3-(aminomethylene)-oxindoles

An efficient palladium-catalyzed protocol for the stereoselective synthesis of 3-(aminoarylmethylene)-oxindoles has been developed. In this approach, Ugi-4-component reaction adducts were used as starting materials for carbopalladative cyclization-Buchwald reaction sequences.     

A simple flow injection spectrophotometric determination of nitrite based on its reaction with thiourea.

A simple flow injection spectrophotometric method for the determination of nitrite is described. Nitrite injected into the flow system reacts with thiourea in acidic medium and the generated thiocyanate ion reacts with Fe(III) in the reagent solution to produce a highly colored product. The influences of chemical and physical parameters including reagent concentrations, sample volume injected, flow rates of the carrier and reagent solutions, reaction coil length and reaction temperature, were studied and optimum values of these parameters were established. Under the optimum conditions, the calibration curve for nitrite was linear over the concentration range 0.36 - 90 microg ml(-1) without preconcentration and over the range 3.8 - 500 ng ml(-1) with a simple online preconcentration step using an anion exchange column. The corresponding detection limits were 0.36 micro ml(-1) and 3.8 ng ml(-1), respectively. Up to 25 samples can be analyzed per hour, with an average relative standard deviation of < or = 1.2%. Interferences by various foreign ions were studied and the method was applied to the determination of nitrite in water and spiked water samples.     

Micellar-catalyzed reactions for flow-injection systems : Determination of pyridoxal

The advantages of applying the solubilization and catalytic properties of aqueous micelle solutions to reactions taking place in flow-injection systems are demonstrated. The reaction of pyridoxal (a B₆ vitamin) with cyanide was investigated in both aqueous and micellar cetyltrimethylammonium bromide (CTAB) solution. Higher sensitivities and lower limits of detection were obtained for the micellar carrier, with the pseudo-first-order reaction rate increasing by a factor of two in 0.05 M CTAB relative to water carrier. Because the micellar aggregates also increase fluorescence quantum yields, use of fluorescence detection gave further signal enhancement, with the limit of detection lowered by a factor of three. Measurement of dispersion in the two systems was also investigated and compared. A new method of characterizing dispersion in flow-injection systems, based on moment analysis of exponentially modified Gaussian peak shapes, is described.     

Solid-phase extraction of Pb2+ ion from environmental samples onto L-AC-Ag-NP by flame atomic absorption spectrometry (FAAS)

The development of a solid-phase extraction (SPE) procedure for the pre-concentration of trace amounts of Pb²⁺ ion on 2-furan-2-yl-1-furan-2-ylmethyl-1H-benzoimidazole loaded on activated carbon modified with silver nanoparticles (L-AC-Ag-NP) was presented. The metal ion retained on the sorbent was quantitatively determined via complexation with the ligand. The complexed metal ion was efficiently eluted using 10 mL of 4 mol L^?1 sulphuric acid in 10 w/v% acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ion were optimised. Using the optimised parameters, the linear response of the SPE method for Pb²⁺ ion were in the ranges of 0.2–160 µg L^?1, and the detection limit for Pb²⁺ ion was 0.034 µg L^?1. The proposed method exhibits a pre-concentration factor (PF) of 80 and an enhancement factor of 30 for Pb²⁺ ion. The presented results demonstrate the successful application of the proposed method for the determination of Pb²⁺ ion in some real samples with high recoveries (>93%) and reasonable relative standard deviation (RSD < 2%).     

Multi-component synthesis of highly substituted imidazoles catalyzed by nanorod vanadatesulfuric acid

Nanorod vanadatesulfuric acid (VSA NRs), as a recyclable and eco-benign catalyst, was used for one-pot synthesis of 2,4,5-trisubstituted imidazoles and 1,2,4,5-tetrasubstituted imidazoles using aldehydes, benzil, benzoin or 9,10-phenanthrenequinone and ammonium acetate or aniline under solvent-free conditions providing high to excellent yields. VSA is easily prepared by a simple reaction of chlorosulfonic acid and sodium metavanadate in high purity. As compared with the conventional procedures, the present protocol offers several advantages such as simplicity of procedure, short reaction time, high yields, easy workup, recoverability and reusability of the catalyst and simple purification of the products.     

On Some Properties of $c$-Frames

In this paper we discuss about $c$-frames, namely continuous frames. Since, $c$-frames are generalizations of discrete frames, we generalize some results of discrete frames to continuous version. We explain some results about relations of projections in Hilbert spaces and $c$-frames to characterize these frames. Also, we will specify (precisely) the synthesis and frame operators of Bochner integrable $c$-frames. Finally, we classify Hilbert-Schmidt operators by $c$-frames and express some new identities for Parseval $c$-frames.     

Multiple solutions for non-homogeneous degenerate Schrödinger equations in cone Sobolev spaces

The present paper deals with the study of semilinear and non-homogeneous Schrödinger equations on a manifold with conical singularity. We provide a suitable constant by Sobolev embedding constant and for p ∈ (2, 2?) with respect to non-homogeneous term g(x) ∈ L ₂ ^n/2 (B), which helps to find multiple solutions of our problem. More precisely, we prove the existence of two solutions to the problem 1.1 with negative and positive energy in cone Sobolev space H _2,0 ^1,n/2 (B). Finally, we consider p = 2 and we prove the existence and uniqueness of Fuchsian-Poisson problem.     

Synthesis of 2-(2-Fluorophenyl)-2-methylamino-Cyclohexanone as a New Ketamine Derivative

The main goal of this article is to the present research on the development of ketamine derivatives. The target molecule was a fluoroderivative of ketamine, for which a multistep synthesis has been reported. This novel ketamine derivative, 2-(2-fluorophenyl)-2-methylamino-cyclohexanone, has been called fluoroketamine by our research group. The starting fluorobenzonitrile was reacted with the appropriate Grignard reagent followed by the bromination reaction to obtain α-bromocyclopentyl-(2-fluorophenyl)-ketone. The reaction of the obtained ketone with methylamine at ?40 °C then resulted in the formation of α-hydroxycyclopentyl-(2-flourophenyl)-N-methylamine. Finally, the five-memberd ring cyclopentanol was expanded to the cyclohexylketone by a thermal rearrangement reaction. The HCl salt of the target molecule, which is soluble in water, was obtained by the acidification of the free fluoroketamine with HCl. Preliminary animal tests on mice have shown that the resulting fluoroketamine has some advantages over ketamine in terms of the effective dose and the recovery time.