Synthesis of Novel Symmetric Porphyrin Schiff Base Dimers by Solid–Liquid Reaction Methodology

A new convenient solid–liquid condensation reaction procedure for the synthesis of novel asymmetric and symmetric meso‐tetraarylporphyrin and metalloporphyrin Schiff bases is reported. The condensation reaction between β‐formyl porphyrin or metalloporphyrins and aromatic amines was carried out at solid–liquid interface by using neutral alumina powder as a solid support for β‐formyl porphyrin or metalloporphyrins and absolute ethanol as the carrier solvent for aromatic amines. Six different asymmetric porphyrin/metalloporphyrin Schiff bases were synthesized via solid–liquid interface reaction methodology. The same solid–liquid synthetic methodology was applied for the synthesis of six novel symmetric Schiff base porphyrin/metalloporphyrin dimers. The comparison of UV–visible spectra of porphyrin Schiff base monomers and dimers revealed that some degree of electronic perturbation has occurred upon dimerization as the Soret bands of the monomers underwent peak broadening along with red shifts. Column chromatography and crystallization were used to purify the compounds. Fourier transform infrared, UV–visible, elemental analysis, ¹H NMR, and mass spectrometry were used to characterize the newly synthesized compounds.     

Development and application of spectrophotometric methods for the determination of citalopram hydrobromide in dosage forms

Study was carried out to develop two simple, fast, accurate and sensitive spectrophotometric methods (A and B) for the determination of citalopram hydrobromide in commercial tablet formulations. In method A, UV spectrophotometer determined the contents of citalopram hydrobromide in tablets at 240 nm in methanol solvent. The linear range was 5-40 microg ml-1 with molar absorptivity 1.4x10(4) l mol-1 cm-1. While the method B based on the reaction of citalopram base as n-electron donor with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone as pi-acceptors to give highly colored complex species that absorb maximally at 590 nm. Beer's law was obeyed in the concentration limit of 10-250 microg ml-1 with molar absorptivity 3.3x10(3) l mol-1 cm-1 for citalopram hydrobromide. The limits of detection and limit of quantification was calculated and found to be 5.2 microg ml-1 and 17.4 microg ml-1 respectively. The proposed methods were found to be rapid, accurate, precise and sensitive for the determination of citalopram hydrobromide in commercial tablet formulations with out interferences from common additives encountered.     

CFD analysis of an oscillating wing at various reduced frequencies

The effect of various reduced frequencies has been examined for an oscillating aspect ratio 10 NACA 0015 wing. An unsteady, compressible three‐dimensional (3D) Navier–Stokes code based on Beam and Warming algorithm with the Baldwin–Lomax turbulence model has been used. The code is validated for the study against published experimental data. The 3D unsteady flow field is simulated for reduced frequency values of 0.1, 0.2 and 0.3 for a fixed mean angle of attack position and fixed amplitude. The type of motion is sinusoidal harmonic. The force coefficients, pressure distributions and flow visualization show that at the given conditions the flow remains attached to the wing surface even at high angles of attack with no clear separation or typical light‐to‐deep category of dynamic stall. Increased magnitude of hysteresis and higher gradients are seen at higher reduced frequencies. The 3D effects are even found at midspan locations. In addition, the rate of decrease in lift near the wing tips compared with the wing root is not much like in the static cases. Copyright © 2008 John Wiley & Sons, Ltd.     

The spin coherence relaxation in the rotating frame as a microscopy parameter for strongly coupled spin systems.

The transverse relaxation time in the rotating frame T2rho is proposed as an effective parameter to get specific contrast in solid state imaging. Several peculiarities make T2rho an interesting candidate to map dynamics and structure in solids: the effect of the secular spin interaction can be controlled by the experimenter and therefore the relaxation associated with the nonsecular terms, which is particularly sensitive to very slow dynamics, can be observed. In this paper we present preliminary results obtained on polymers and prove the capability of the MARF Imaging, enhanced by a filter based on rotary echo refocusing, to produce images of solids contrasted by T2rho.     

Copper(I) and silver(I) complexes of 1,5-methylene- and diethylmethylene-bridged bis(oxazoline) ligands. In situ Cu(II)-catalyzed oxidation of methylene bridge

Silver(I) and copper(I) complexes of C₂-symmetric bis(oxazoline) ligands were studied by UV, NMR, IR, EPR and ES-MS spectroscopies. The stability constants of the Ag-1a and Ag-1b complexes with 1:1 and 1:2 stoichiometries in acetonitrile were determined by NMR spectrometric titrations. The evidence of tetrahedral coordination for complex (Ag(1a)₂(⁺ was obtained from the complexation induced shifts (CIS) and NOEs. Mass spectra revealed the Cu(II) mediated oxidation of methylene bridge in copper complexes of 1a and 1b, which was in accordance with the UV, NMR, IR and EPR findings. The efficiency of Cu(I) complexes of methylene-bridged 1,5-bis(oxazoline)s 1 as chiral catalysts in stereoselective cyclopropanation of styrene with ethyl diazoacetate, was compared to that of the dialkylmethylene-bridged 1,5-bis(oxazoline)s 2.     

Exploring Amantadine Derivatives as Urease Inhibitors: Molecular Docking and Structure–Activity Relationship (SAR) Studies

This article describes the design and synthesis of a series of novel amantadine-thiourea conjugates (3a–j) as Jack bean urease inhibitors. The synthesized hybrids were assayed for their in vitro urease inhibition. Accordingly, N-(adamantan-1-ylcarbamothioyl)octanamide (3j) possessing a 7-carbon alkyl chain showed excellent activity with IC₅₀ value 0.0085 ± 0.0011 µM indicating that the long alkyl chain plays a vital role in enzyme inhibition. Whilst N-(adamantan-1-ylcarbamothioyl)-2-chlorobenzamide (3g) possessing a 2-chlorophenyl substitution was the next most efficient compound belonging to the aryl series with IC₅₀ value of 0.0087 ± 0.001 µM. The kinetic mechanism analyzed by Lineweaver–Burk plots revealed the non-competitive mode of inhibition for compound 3j. Moreover, in silico molecular docking against target protein (PDBID 4H9M) indicated that most of the synthesized compounds exhibit good binding affinity with protein. The compound 3j forms two hydrogen bonds with amino acid residue VAL391 having a binding distance of 1.858 Å and 2.240 Å. The interaction of 3j with amino acid residue located outside the catalytic site showed its non-competitive mode of inhibition. Based upon these results, it is anticipated that compound 3j may serve as a lead structure for the design of more potent urease inhibitors.     

Recent trends in ring opening of epoxides by amines as nucleophiles

β-Amino alcohols are versatile intermediates in the synthesis of various biologically potent compounds, which can also be achieved by ring opening of epoxides by amines. In the present review, focus has been placed on the ring opening of epoxides with amines under a variety of reaction parameters reported during 2011–2015. All the factors that resulted in excellent yields and high regioselectivity, are environmentally benign, and use mild conditions have been discussed in detail. In addition, the applications of these methods in the synthesis of biologically active compounds such as β-blockers have also been described.     

Sobolev gradient approach for the time evolution related to energy minimization of Ginzburg–Landau functionals

The Sobolev gradient technique has been discussed previously in this journal as an efficient method for finding energy minima of certain Ginzburg–Landau type functionals [S. Sial, J. Neuberger, T. Lookman, A. Saxena, Energy minimization using Sobolev gradients: application to phase separation and ordering, J. Comput. Phys. 189 (2003) 88–97]. In this article a Sobolev gradient method for the related time evolution is discussed.     

Haloxylines A and B, antifungal and cholinesterase inhibiting piperidine alkaloids from Haloxylon salicornicum

Haloxylines A (1) and B (2), new piperidine alkaloids, have been isolated from the chloroform soluble fraction of Haloxylon salicornicum and their structures elucidated by spectroscopic techniques including 2D-NMR. Both the compounds displayed antifungal and cholinesterase enzymes inhibitory potentials.     

Excitations in randomly diluted two-dimensional ferromagnets

The dynamics of a randomly diluted Heisenberg ferromagnet on a two-dimensional square lattice is calculated using a CPA procedure introduced by Theumann and Tahir-Kheli. The density of states and frequency-wave-vector-dependent response functions at various symmetry points of the Brillouin zone are presented for several magnetic concentrations. Our results for the density of states are compared with those obtained from computer-experiment calculations of Huber and are found to be in good agreement with them. The spin-wave stiffness coefficient is calculated, and comparison is made with results on two-dimensional resistor networks given by Watson et al.