Preparation,molecular definition,spectroscopic characterization and density functional theory calculations on N’-(4-(3-methyl-3-phenylcyclobutyl)-3-phenylthiazol-2(3H)-ylidene)benzenesulfonohydrazide

Abstract

A new sulfonyl derivative (C₂₆H₂₅N₃O₂S₂), N’-(4-(3-methyl-3-phenylcyclobutyl)?3-phenylthiazol-2(3H)-ylidene)benzenesulfonohydrazide, was prepared from a mixture of benzenesulfonylhydrazide and phenylisothiocyanate in ethanol. The 3?D crystal structure, unit-cell dimensions, space group and crystal system of compound were investigated by single-crystal X-ray diffraction (SCXRD). FT-IR spectrum in solid state was observed in the region 4000–400?cm^?1 and the ¹H and ¹³C NMR spectra were recorded in CDCl₃ solution. In order to support the experimental results, the molecular geometry, vibrational frequencies, ¹H and ¹³C chemical shifts in the ground state have been calculated by using the density functional method (DFT/B3LYP) together with 6-311?G+(d, p) basis set. A good linear correlation between experimental and theoretically predicted structural and spectral parameters was observed (R²～0.9).     

The first tris(saccharinato) complexes. Syntheses, spectral, thermal and structural characterization of ApyH[Cu(N–sac)2(O–sac)(H2O)2] and ApyH[Zn(N–sac)3- (H2O)] (ApyH=2–aminopyridinium and sac=saccharinate)

The reaction of the Schiff base salicylideneaminopyridine with [M(sac)₂(H₂O)₄] · 2H₂O, where M is copper(II) or zinc(II), and sac is the saccharinate anion, results in the formation of the new tris(saccharinato) complexes ApyH[Cu(N-sac)₂ (O-sac)(H₂O)₂] (1) and ApyH[Zn(N-sac)₃(H₂O)] (2), which have been characterized by elemental analyses, magnetic measurements, FT-IR spectroscopy, thermal analysis and X-ray diffraction. The Schiff base did not coordinate to the metal ions, but decomposed during the reaction, forming a 2-aminopyridinium cation ApyH, which remained outside the coordination sphere as a counter ion. (1) and (2) are the first examples of mononuclear tris(saccharinato) complexes of copper(II) and zinc(II). Both complexes are isomorphous with the triclinic space group P-1, (1) consisting of an ApyH cation and a [Cu(sac)₃(H₂O)₂]^– anion in which the copper(II) ion has trigonal bipyramidal surroundings. The sac ligands in (1) exhibit unusual and non-equivalent coordination, behaving as ambidentate ligands. One of them coordinates to the metals through the carbonyl oxygen atom, while the other two sac ligands are bonded to the metals via the imino nitrogen atom. The zinc(II) ion in (2) is tetrahedrally coordinated by three N-donor sac ligands and an aqua ligand. The crystal structures of (1) and (2) are stabilized by intermolecular hydrogen bonds and aromatic – stacking interactions.     

Some Relations on the Double $$mathcal {L}_{22}$$ -Integral Transform and Their Applications

Mediterranean Journal of Mathematics - A variant of the Jensen–Mercer operator inequality is proved for a superquadratic function and positive linear operators on a Hilbert space using a...     

The synthesis,characterization and effect of molar mass distribution on solid-state degradation kinetics of oligo(orcinol)

Journal of Thermal Analysis and Calorimetry - In this study, the oxidative polymerization of orcinol monohydrate using different oxidants such as NaOCl, H2O2, and air was investigated....     

Nanojet impingement cooling of an isothermal surface in a partially porous medium under the impact of an inclined magnetic field

Journal of Thermal Analysis and Calorimetry - In this study, jet impingement heat transfer characteristics for a layered nanofluid and porous domains under the effects of inclined uniform magnetic...     

Accurate and simple determination of oxcarbazepine in human plasma and urine samples using switchable-hydrophilicity solvent in GC–MS

This work presents a sensitive and rapid analytical method for the determination of oxcarbazepine in human plasma and urine samples. A vortex-assisted switchable hydrophilicity solvent-based liquid phase microextraction (VA–SHS–LPME) was used to preconcentrate oxcarbazepine from the samples before the determination by gas chromatography mass spectrometry. The switchable hydrophilicity solvent was synthesized by protonating N,N-dimethylbenzylamine with carbon dioxide to make it totally miscible with an equivalent volume of water. Parameters of the VA–SHS–LPME method including volume of switchable hydrophilicity solvent, concentration/volume of sodium hydroxide and vortex period were systematically optimized. Under the optimum conditions, good linearity ranging from 27.03 to 353.47 μg/kg was obtained for the analyte. Limit of detection and quantitation values were found to be 6.2 and 21 μg/kg (mass base), respectively. The relative standard deviation was calculated as 6.9% for six replicate measurements of the lowest concentration of the calibration plot. Satisfactory recovery results were calculated in the range of 97–100% for human plasma and urine samples spiked at five different concentrations.     

Direct Constructions for General Families of Cyclic Mutually Nearly Orthogonal Latin Squares

Two Latin squares and , of even order n with entries , are said to be nearly orthogonal if the superimposition of L on M yields an array in which each ordered pair , and , occurs at least once and the ordered pair occurs exactly twice. In this paper, we present direct constructions for the existence of general families of three cyclic mutually orthogonal Latin squares of orders , , and . The techniques employed are based on the principle of Methods of Differences and so we also establish infinite classes of “quasi‐difference” sets for these orders.     

The effect of the oxidant used during polymerization on the solid-state decomposition kinetics of poly(4-methyl catechol)

Herein, the oxidative polymerization of 4-methyl catechol using different oxidants including NaOCl, H₂O₂, and air were reported. Potassium hydroxide solution was used as the reaction solvent and polymerization studies were carried out between 323 and 363 K. Optimum reaction conditions of the polymerization were established and NaOCl was found as the most active oxidant. The structure and characterization of the polymer using FT-IR, ultraviolet–visible (UV–Vis), ¹H-NMR, ¹³C-NMR, thermogravimetry and size exclusion chromatography were confirmed. In addition, the relationship between molar mass distribution of polymer and kinetics parameters such as activation energy, pre-exponential factor of decomposition process was investigated. For this purpose, methods based on multiple heating rates such as Flynn–Wall–Ozawa, Friedman, Tang, Kissinger–Akahira–Sunose, and Kissinger were used. The results obtained show that activation energy increased with an increase of molar mass.     

A practical synthesis of novel α-dibromoalkyl- and trimethylsilylmethyl-aminoboranes and derivatives

Addition of LDA to a mixture of trimethylborate and dibromomethane in THF at a temperature of -78°C leads to the formation of dibromomethyllithium and its capture by borate ester. ClB(OMe)(2) converts the resulting borate salt to dimethoxy(dibromomethyl)borane 2. N,N-Dimethylamino(methoxy)(dibromomethyl)borane 3 and N,N-bis(dimethylamino)(dibromomethyl)borane 4 were prepared by an amination reaction between N,N-dimethylaminotrimethylsilane and dimethoxy(dibromomethyl)borane 2. To obtain dichlorotrimethylsilylmethylborane 7 not containing the α-halomethyl group, N,N-bis(dimethylamino)(trimethylsilylmethyl)borane 5 was first obtained from the reaction of ClB(NMe(2))(2) with an organolithium reagent. Dimethoxy(trimethylsilylmethyl)borane 6 was then prepared by methoxylation of compound 5. Finally, compound 7 was prepared by chlorination of 6 using BCl(3). The chemical structures of these compounds were determined using (13)C, (1)H, (11)B NMR and GC/MS/MS techniques.