Catalytic carbonylation for the synthesis of chemical intermediates

Chemistry related to three catalytic carbonylation reactions is discussed. Synthesis of diphenylurea from nitrobenzene, aniline, and CO gives isolated yields above 98% at 100–120 °C and 15–60 bar of CO in the presence of a palladium (II) complex, PPh₃ and NEt₄Cl. Experimental evidence was provided to prove a new reaction stoichiometry and involvement of a carbamoyl intermediate. In carbonylation of HCHO over ion exchange resin catalysts, reaction temperature, time, pressure, and solvent were important variables to obtain high yields of methyl glycolate. Carbonylation of isobutylphenylethanol at 120°C and 40 bar of CO in the presence of PdCl₂−PPh₃−HCl gives 98% yield of α-(4-isobutylphenyl) propionic acid (ibuprofen). Each catalyst component had a definite role that is indispensable for an efficient overall reaction.     

Chemical modification of silica gel with synthesized Schiff base hydrazone derivative and application for preconcentration and separation of U(VI) ions from aqueous solutions

Schiff base hydrazone derivative (HL) sorbent was synthesized according to the literature to be used in the adsorption and preconcentration of U(VI) ions from aqueous solution and it was exposed to immobilization, and new solid support material was obtained. For this purpose, Schiff base hydrazone derivative (HL) was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane, then analyzed by Fourier transform infrared, Brunauer–Emmett–Teller, scanning electron microscopy and elemental analysis. The influence of the solution pH, amount of sorbent, contact time, temperature, foreign ion effect and initial U(VI) concentration was investigated. The maximum U(VI) uptake capacity was found to be 8.46 mg/g.     

Investigation of the behavior of an Ising metamagnet under the influence of a field using Glauber dynamics

In this study, the kinetics of the Ising metamagnet where the interlayer interactions are ferromagnetic has been investigated under the mean field approximation. In describing the kinetics of the system, Glauber stochastic dynamics in the presence of an external field which performs time-dependent oscillations, has been utilized. Obtained results could be identified by two distinct types: the asymmetric solutions oscillating in the vicinity of finite values where the lattice magnetization has different values and the symmetric solutions being zero where the sublattice magnetizations are equal to each other. On the other hand, it has been observed that in the case where the system's initial state has a homogenous magnetization it exhibits two different periodical behaviors in the course of time.     

A switchable ionic liquid with polarity swing-assisted regeneration properties used for the preconcentration of cadmium in biological samples

In the present study the cadmium (Cd) was determined in serum samples of psoriatic patients. The severity of psoriasis was evaluated according to criteria based on standard clinical diagnosis using Psoriasis Area Severity Index (PASI) score. In present study, an innovative tunable green solvent system based microextraction (TSS-ME) was applied for the enrichment of Cd in acid digested serum samples prior to determination with flame atomic absorption spectrometry. The hydrophobic complex of Cd-ammonium pyrrolidine thiocarbamate was extracted in a tunable solvent system which was prepared from a polybasic amine (N, N, N′, N′-tetramethyl-1, 4-diaminobutane), decanol and water system. The tunable green solvent system (TSS) which has zero ionic strength was converted to homogeneous monophasic polar hydrophilic phase via exposure to CO₂ at different pressure and time duration. Then hydrophobic enriched Cd- ammonium pyrrolidine thiocarbamate was back extracted, using HNO₃ (0.1 to 0.5 mol L⁻¹) then the second round of TSS-ME was applied. The acidic aqueous phase enrich with analyte was separated from tunable solvent. The separated TSS was easily reused for up to 10 time for preconcentration purposes without loss of its enrichment character. The smoker and nonsmoker psoriatic patients at PASI >10, have two to three folds higher Cd levels in serum samples than healthy persons.     

Electroreduction of Derivatives of N,N'-Dioxides of Phenazine and Quinoxaline in Nonaqueous Media and in the Presence of Proton Donors of Medium Strength

Russian Journal of Electrochemistry - The electroreduction (ER) of benzo[a]phenazine-7,12-dioxide (1) and 2-ethoxycarbonyl-3-methyl-quinoxaline-1,4-dioxide (2) in DMF on a glassy carbon electrode...     

A new 14-membered cyclopeptide alkaloid from Zizyphus oxyphylla

One new 14-membered frangulanine-type cyclopeptide alkaloid, oxyphyl line-A (1) has been isolated from the stem bark of Zizyphus oxyphylla together with the known 13-membered cyclopeptide, nummularine R (2). The structure was established on the basis of spectral studies particularly 2D NMR.     

The effect of competition between the frequency of the field and the frequency of the spin flipping on the kinetics of Ising metamagnet

We consider the effect of a variable representing the competition between the frequency of the field and the frequency of the spin flipping (Ω) on the dynamics of the metamagnetic Ising model in a cubic lattice under the presence of a time varying (oscillating) external magnetic field. The system is modelled with a formalism of master equation at a mean-field level. The time averaged staggered magnetization (Ms) acts as the order parameter and divides temperature field plane into three regions: anti-ferromagnetic, paramagnetic and coexistence of anti-ferromagnetic and paramagnetic phases. It is observed that the topology of the dynamical phase diagram depends strongly on Ω as well as the ratio between interlayer and intralayer couplings.     

Structural,magnetic and electrical properties of Co1−xZnxFe2O4 synthesized by co-precipitation method

Nanoparticles of Co_1−xZn_xFe₂O₄ with stoichiometric proportion (x) varying from 0.0 to 0.6 were prepared by the chemical co-precipitation method. The samples were sintered at 600 °C for 2 h and were characterized by X-ray diffraction (XRD), low field AC magnetic susceptibility, DC electrical resistivity and dielectric constant measurements. From the analysis of XRD patterns, the nanocrystalline ferrite had been obtained at pH=12.5–13 and reaction time of 45 min. The particle size was calculated from the most intense peak (3 1 1) using the Scherrer formula. The size of precipitated particles lies within the range 12–16 nm, obtained at reaction temperature of 70 °C. The Curie temperature was obtained from AC magnetic susceptibility measurements in the range 77–850 K. It is observed that Curie temperature decreases with the increase of Zn concentration. DC electrical resistivity measurements were carried out by two-probe method from 370 to 580 K. Temperature-dependent DC electrical resistivity decreases with increase in temperature ensuring the semiconductor nature of the samples. DC electrical resistivity results are discussed in terms of polaron hopping model. Activation energy calculated from the DC electrical resistivity versus temperature for all the samples ranges from 0.658 to 0.849 eV. The drift mobility increases by increasing temperature due to decrease in DC electrical resisitivity. The dielectric constants are studied as a function of frequency in the range 100 Hz–1 MHz at room temperature. The dielectric constant decreases with increasing frequency for all the samples and follow the Maxwell–Wagner's interfacial polarization.