Synthesis,crystal structures,characterization and antimicrobial activities of 5-hydroxyisophthalate complexes

Two 5-hydroxyisophthalate complexes of nickel(II), formulated as [Ni(μ-Hhip)(2-hepy)₂] _n (1) and [Ni₂(μ-Hhip)₂(dap)₄] _n (2) (H₃hip = 5-hydroxyisophthalic acid, 2-hepy = 2-(2-hydroxyethyl)pyridine, dap = 1,3-diaminopropane), have been synthesized and characterized by chemical and spectroscopic methods. The molecular structures of the complexes have been determined by single-crystal X-ray diffraction analysis. The Ni(II) centres have distorted octahedral geometries in both crystals. Furthermore, both complexes have 1D chain structures in which the individual chains are linked together via hydrogen bonds to give 3D frameworks. Evaluation of the complexes by the agar diffusion method showed that they have weak antibiotic activities against the tested microorganisms.     

Second‐order backward stochastic differential equations and fully nonlinear parabolic PDEs

For a d‐dimensional diffusion of the form dX_t = μ(X_t)dt + σ(X_t)dW_t and continuous functions f and g, we study the existence and uniqueness of adapted processes Y, Z, Γ, and A solving the second‐order backward stochastic differential equation (2BSDE) If the associated PDE has a sufficiently regular solution, then it follows directly from Itô's formula that the processes solve the 2BSDE, where ?? is the Dynkin operator of X without the drift term. The main result of the paper shows that if f is Lipschitz in Y as well as decreasing in Γ and the PDE satisfies a comparison principle as in the theory of viscosity solutions, then the existence of a solution (Y, Z,Γ, A) to the 2BSDE implies that the associated PDE has a unique continuous viscosity solution v and the process Y is of the form Y_t = v(t, X_t), t ∈ [0, T]. In particular, the 2BSDE has at most one solution. This provides a stochastic representation for solutions of fully nonlinear parabolic PDEs. As a consequence, the numerical treatment of such PDEs can now be approached by Monte Carlo methods. © 2006 Wiley Periodicals, Inc.     

Special Issue: Optimization and Stochastic Control in Finance,Journal of Optimization Theory and Applications

In this paper, we study the near-optimal control for systems governed by forward–backward stochastic differential equations via dynamic programming principle. Since the nonsmoothness is inherent in this field, the viscosity solution approach is employed to investigate the relationships among the value function, the adjoint equations along near-optimal trajectories. Unlike the classical case, the definition of viscosity solution contains a perturbation factor, through which the illusory differentiability conditions on the value function are dispensed properly. Moreover, we establish new relationships between variational equations and adjoint equations. As an application, a kind of stochastic recursive near-optimal control problem is given to illustrate our theoretical results.     

A sensitive spectrofluorimetric method for the determination of ranitidine hydrochloride in pharmaceutical preparation

A simple, precise and sensitive spectrofluorimetric method was developed and validated for the determination of ranitidine in pharmaceutical preparations. The method is based on derivatization of ranitidine with 4-fluoro-7-nitrobenzofurazan (NBD-F). The method was successfully validated in accordance to ICH guidelines. The validation characteristics included linearity, limit of detection, limit of quantification, accuracy, precision, specificity and robustness. The method is linear over the range of 40?C1200 ng/mL. The recoveries were ranged from 98.97 to 99.43%. The proposed method was applied for the determination of ranitidine in commercially available tablets. The results were compared with those obtained by reference method using t and F-tests.     

Application of Supermacroporous Monolithic Hydrophobic Cryogel in Capturing of Albumin

Supermacroporous poly{2-hydroxyethyl methacrylate-co-[N,N-bis(2,6-diisopropylphenyl)-perylene-3,4,9,10-tetracarboxylic diimide]} [poly(HEMA-co-DIPPER)] monolithic cryogel column was prepared by radical cryocopolymerization of HEMA with DIPPER as functional comonomer and N,N′-methylene-bisacrylamide (MBAAm) as crosslinker directly in a plastic syringe for adsorption of albumin. The monolithic cryogel contained a continuous polymeric matrix having interconnected pores of 10–50 μm size. Poly(HEMA-co-DIPPER) cryogel was characterized by swelling studies, FTIR, scanning electron microscopy, and elemental analysis. The equilibrium swelling degree of the poly(HEMA-co-DIPPER) cryogel was 14.7 g H₂O/g dry cryogel. Poly(HEMA-co-DIPPER) cryogel was used in the adsorption/desorption of albumin from aqueous solutions. The nonspecific adsorption of albumin onto plain poly(HEMA) cryogel was very low (3.36 g/g polymer). The maximum amount of albumin adsorption from aqueous solution in acetate buffer was 40.9 mg/g polymer at pH 5.0. It was observed that albumin could be repeatedly adsorbed and desorbed with the poly(HEMA-co-DIPPER) cryogel without significant loss of adsorption capacity.     

Synthesis,spectroscopic characterization and X-ray single crystal structures of trans-bis[4-methoxyphenyl (3-methylbutyl) dithiophosphinato] nickel(II) and bis [4-methoxyphenyl (3-methylbutyl) dithiophosphinato]cobalt(II) complexes

Thionation of 3-methylbutylmagnesium bromide with Lawesson’s Reagent (LR) gave 4-methoxyphenyl (3-methylbutyl)dithiophosphinic acid (DTPA), and the latter was converted to the ammonium salt (NH₄L = Ammonium 4-methoxyphenyl (3-methylbutyl) dithiophosphinate). The complex, trans–bis[4-methoxyphenyl(3–methylbutyl) dithiophosphinato] nickel(II) [NiL₂], was prepared by the reaction of NH₄L with NiCl₂.6H₂O in EtOH. Bis [4-methoxyphenyl (3-methylbutyl) dithiophosphinato]cobalt(II) [(CoL₂)₂] was also prepared in the same way. The structures of the complexes have been characterized by elemental analysis, FTIR, ¹H, ¹³C, ³¹P NMR and X-ray diffraction. The single crystal X-ray structures of [NiL₂] and [(CoL₂)₂] show that the nickel complex is square planar while the cobalt counterpart has tetrahedral coordination with a dimeric structure. Bond lengths, angles, torsion angles and dihedral angles are correlated to the structures and also compared with the literature data on similar compounds.     

Synthesis,crystal structure,HF and DFT calculations of 1-(2-chlorobenzyl)-N-(1-(2-chlorobenzyl)-4,5-dihydro-1H-imidazol-2-yl)-1H-benzimidazol-2-amine

The titled compound (1), has been synthesized and characterized by IR and ¹H-NMR spectroscopy, and single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P-1. The crystal structure is stabilized by C-H…π and aromatic π-π interactions. There are also intramolecular N-H…N and C-H…N hydrogen bonds in the molecule. The use of quantum chemical calculations to characterise and optimise the choice of material is illustrated by ab initio treatments. Vibrational frequencies and LUMO-HOMO energy difference of 1 have also been investigated by Density functional theory (DFT) and Hartree-Fock (HF) calculations. Calculated frequencies are in good agreement with the corresponding experimental data.     

X-Ray diffraction and vibrational spectroscopic study of 2-chloro-N-{4-[3-(2,5-dimethylphenyl)-3-methylcyclobutyl]-thiazol-2-yl}-acetamide

The title compound C₁₈H₂₁ClN₂SO crystallizes with Z = 4 in space group P2₁/c. The structure of the title compound was characterized by ¹H-NMR, ¹³C-NMR, IR and single crystal diffraction. There are an intermolecular N-H…O hydrogen bond and a C-H…π interactions in crystal packing. In addition to the molecular geometry and packing obtained from X-ray experiment, the molecular geometry and vibrational frequencies of the title compound in ground state have been calculated using density functional theory method DFT (B3LYP) with 6-31G (d, p) basis set. Calculated frequencies, bond lengths, angles and dihedral angles are in good agreement with the corresponding experimental data.     

Investigation of thin-layer chromatography properties of some transition metal complexes based on ditiocarbamates

Sodium diethyldithiocarbamate (DEDTC) and ammonium pyrolidinedithiocarbamate (PyDTC) are prepared as their Co or Cu (M) complexes [M(DEDTC)(2) and M(PyDTC)(2), respectively]. The complexes are prepared by reactions of DEDTC and PyDTC with metal (II) nitrates, and they are examined for chromatographic properties using thin-layer chromatography systems. These complexes and their mixtures are spotted on the activated and non-activated 250-microm thick thin layers of commercial silica gel (Si-60GF(254)). Pure toluene and a toluene-cyclohexane mixture (3:1, v/v) are used as mobile phases for running the complexes. These chromatographic systems are successfully used for the qualitative analysis of the corresponding metal cations and the separation of components in both M(DEDTC)(2) and M(PyDTC)(2) complex mixtures. In addition, non-activated layers are more successful than activated layers. This study may be useful in understanding the effects of stationary and mobile phase properties, retention mechanisms, and the effects of the nature of metal and ligand type on the chromatographic behavior and parameters [e.g., retention factors, theoretical plate numbers, and resolution] of the complexes.