Characterized Using Elemental Analysis Research Articles

Synthesis, characterization and anticancer activity of Ni(II), Cu(II), Pd(II) and Au(III) complexes derived from novel Mannich base

AbstractNew four complexes of Ni(II), Cu(II), Pd(II), and Au(III) were derived from the tridentate ligand 3‐((3‐(4‐hydroxyphenyl)‐5‐mercapto‐4H‐1,2,4‐triazol‐4‐yl)(3‐oxobutyl)amino)naphtho[2,3‐b]furan‐2(3H)‐one (L), which synthesized using condensation reaction of formaldehyde, acetone, and secondary amine (Mannich reaction). The secondary amine is a heterocyclic compound possesses two rings, naphthafuran and triazole, both rings prepared through intermolecular cyclization reactions. Considering that naphthafuran‐2‐one derived from α‐amino nitrile. The α‐amino nitrile compound contains the other triazole ring which illustrated to the structure through successive steps. The compounds were characterized using elemental analysis (C.H.N.S), FT‐IR, ultraviolet–visble spectroscopy, thermal gravimetric analysis (TGA), flame atomic absorption, molar conductivity, and magnetic susceptibility measurements. Accordingly, the probable geometries of the complexes were suggested as square planner, and they have electrolytic nature. Thus, chemical formula; [NiLCl]Cl·6H2O, [CuLCl]Cl·2H2O, [PdLCl]Cl·2H2O, and [AuLCl]Cl2·3H2O. Cytotoxic effect was studied on brain cancer cell line (AMJM cell line) at different concentrations for L and complexes. The results showed that gold(III) complex has the highest cytotoxicity among all compounds.

Spectroscopic investigation, molecular structure, catalytic activity with computational studies of a novel Pd(II) complex incorporating unsymmetrical tetradentate Schiff base ligand

The treatment of an unsymmetrical tetradentate Schiff base ligand with Pd(OAc)2 salt yields novel palladium(II) Schiff base complex. The generated palladium(II) complex was characterized using elemental analysis (CHN) and different spectroscopic methods such as FT-IR and 1H NMR. Single crystal X-ray diffraction (SC-XRD) investigation has also been used to examine the crystal structure of the palladium complex. It is revealed from the SC-XRD study that the palladium ion in the complex is tetra-coordinated, inhabited by ONNO donor sites of the chelated ligand in a distorted square planar manner. The non-covalent interactions were explored by Hirshfeld surface analysis. The theoretical parameters calculated by DFT using the B3LYP/Def2-TZVP level of theory revealed that the theoretical conclusions matched the actual findings. For different aryl halides, the palladium(II) complex has exhibited excellent efficiency in the Suzuki-Miyaura cross-coupling reactions (SMCR), yielding biaryls in good to high yield.

Practical and Computational Studies of Bivalence Metal Complexes of Sulfaclozine and Biological Studies.

In the search for novel, metal-based drug complexes that may be of value as anticancer agents, five new transition metal complexes of sulfaclozine (SCZ) with Cu(II), Co(II), Ni(II), Zn(II), and Fe(II) were successfully synthesized. The chemical structure of each complex was characterized using elemental analysis (CHN), IR spectroscopy, UV–Vis spectroscopy, thermogravimetric analysis (TGA), and electronic paramagnetic resonance (EPR) spectroscopy. IR spectra indicated that the donor atoms were one sulfonyl oxygen atom and one pyrazine nitrogen atom, which associated with the metal ions to form a stable hexagonal coordination ring. The metal–ligand stability constant (Kf) revealed that Cu(II) and Ni(II) have good coordination stability among the metal compounds. Theoretical studies using DFT/B3LYP were performed to further validate the proposed structures. The obtained results indicated that Cu(II) has a trigonal bipyramidal geometry, whereas Fe(II), Co(II), and Ni(II) have an octahedral structure, while Zn(II) has a tetrahedral arrangement. The bio-activities of the characterized complexes were evaluated using DNA binding titration and molecular docking. The binding constant values for the metal complexes were promising, with a maximum value for the copper metal ion complex, which was 9 × 105 M-1. Molecular docking simulations were also carried out to evaluate the interaction strength and properties of the synthesized metal complexes with both DNA and selected cancer-relevant proteins. These results were supported by in vitro cytotoxicity assays showing that the Cu(II) and Ni(II) complexes display promising antitumor activity against colon and breast cancer cell lines.

Biological properties of chitosan derivatives associated with the ceftazidime drug

Chitosan has become promising as a biomaterial because of its biocompatible, biodegradable nature and non-toxic. The biochemical and antioxidant properties of chitosan modified with acetylacetone and ethylenediamine (Cacen) or diethylenetriamine (Cacdien) associated with ceftazidime (F) were investigated. Chitosan was characterized using Elemental Analysis (CHN), Thermal Analysis (TG/DTG/DSC), X-Ray Diffractometry (XRD), and was investigated an in vitro hemolytic cytotoxicity test, Artemia saline larvae for toxicity and in vitro antioxidant activity by DPPH (2,2-diphenyl-1-picrylhydrazyl). The chemical modification was confirmed by CHN, XRD and TG. The Cacen, Cacdien, CacenF and CacdienF derivatives presented high percentages of nitrogen (7.6%, 7.9%, 14.1% and 19.2%, respectively), confirming the modification and drug adsorption. The average molecular weight of chitosan and its derivatives were 132 kDa, with very few variations after modification. This incorporation decreased in the crystallinity index of Cacen (7.1%) and Cacdien (4.3%), as well as the incorporation of the drug (CacenF 0.3% and CacdienF 3.4%). FTIR spectra showed bands at 1580–1654 cm−1 referring to carbonyl and imine group and bands at 3500–3300 and 1462–1264 cm−1 related to vibration and deformation the amine group. 13C NMR spectroscopy was observed new peaks in carbonyl and imine regions (170–200 ppm). The thermal stability of the derivatives without the drug improved according to TG/DTG/DSC analysis, however there were decreased in the derivatives with the drug. The biocompatibility of the derivatives was confirmed by the low hemolytic rate (<5%), non-toxic on Artemia salina (LD50%>3000 ppm), and significant index (1–34%) of antioxidant activity. The results demonstrated that chitosan and its derivatives are promising biomaterials.

Quantitative Sensitization Efficiencies in NIR-Emissive Homoleptic Ln(III) Complexes Using 2-(5-Methylpyridin-2-yl)-8-hydroxyquinoline.

A series of isostructural lanthanide complexes [Ln(MPQ)3] (Ln = Nd, Gd, Er, Yb, Lu) using a monoanionic tridentate methylpyridyl-substituted 8-hydroxyquinoline ligand (MPHQ = 2-(5-methylpyridin-2-yl)-8-hydroxyquinoline) have been prepared and characterized using elemental analysis (CHN), single-crystal X-ray diffraction (XRD), and 1H NMR spectroscopy. This ligand forms homoleptic charge-neutral lanthanide complexes with three coordinated ligands arranged in an "up-up-down" fashion around the metal center. The photophysical properties of the Nd, Er, and Yb complexes were investigated using absorption and emission spectroscopy, with the latter species displaying efficient sensitization in the Near Infra-Red (NIR) region and a photoluminescence quantum yield (PLQY) as high as 1.0% in CH2Cl2 solution. The intersystem crossing and energy-transfer processes involved in the antenna effect were further investigated using transient absorption techniques, which revealed essentially quantitative sensitization efficiencies for the NIR-emitting cations.

Synthesis, characterization, anti-ulcer action and molecular docking evaluation of novel benzimidazole-pyrazole hybrids

A series of six novel benzimidazole-pyrazole hybrid molecules was synthesized and characterized using elemental analysis (CHN) and spectroscopic methods (1HNMR, FT-IR). All the synthesized compounds were evaluated for their in vivo anti ulcerogenic activity using Albino rats (weighing 180–220 g). The interactions between the compounds and active site residues of H+/K+ ATPase were investigated by molecular docking studies using autodock vina 4.0. SCH28080 was used to validate the docking results. Also the drug likeliness of these compounds was predicted using Molinspiration server in light of Lipinski’s rule of five. All the six synthesized compounds exhibited higher anti-ulcer activity as compared to omeprazole. These novel hybrid compounds showed comparable anti-ulcer potential of 72–83% at dose level of 500 µg/kg, whereas omeprazole showed 83% anti-ulcer activity at dose level of 30 mg/kg. The results clearly indicate that these novel benzimidazole-pyrazole hybrids can present a new class of potential anti ulcer agents and can serve as new anti-ulcer drugs after further investigation.Graphical abstractAn overveiw of synthesis, in silico and in vivo antiulcer screening of benzimidazole pyrazole hybrids

Synthesis of succinimide based novel additives for viscosity reduction of bituminous binder

Three novel succinimide based additives DDSA-TETA, DDSA-TEPA and DDSA-PEHA were synthesized by a simple refluxing reaction between dodecenylsuccinic anhydride (DDSA) with triethylenetetramine (TETA), tetraethylenepentamine (TEPA) and pentaethylenehexamine (PEHA) respectively in toluene. All were characterized using elemental analysis (CHN), infrared (IR) spectroscopy and nuclear magnetic resonance (NMR) spectroscopy. The compounds were then evaluated as additive in hard base bitumen in order to reduce the viscosity and increase the penetration. Comparatively DDSA-TEPA was found to be most effective in reducing the viscosity and improving the penetration property. It also shows the concentration effect without much affecting the other important physical parameters like softening point and ductility.

Synthesis, characterization and antileishmanial studies of some bioactive heteroleptic pentavalent antimonials

In pursuit of safe drug candidates for the treatment of parasitic diseases like leishmaniasis, a series of heteroleptic pentavalent antimonials of the type [R3Sb(O2CR′)2] (1–9) have been synthesized and characterized using elemental analysis (CHN), Fourier transform infrared spectroscopy and multinuclear (1H and 13C) NMR spectroscopy. The carboxylates studied are predominantly substituted benzoates with some complexes having acetato or nicotinato ligands. The crystal structures of [Sb(C6H5)3(o‐NH2C6H4COO)2] (1) and [Sb(C6H5)3(3,5‐Cl2C6H3COO)2] (4) were determined as essentially monomeric with an Sb(V) centre and shown to adopt geometries intermediate between trigonal bipyramidal and square pyramidal. The antileishmanial activity was assessed against Leishmania tropica KWH23, and also human macrophages were used to measure the cytotoxicity of these complexes. The IC50 of the antimonials 1–9 indicates their efficaciousness as compared with the standard antimonial drug used. The significant activity of complex 1 assumes that greater multitude of interactions is the cause of enhanced antileishmanial activity. Cytotoxicity results showed that these antimonials are highly active even at low concentrations and are biocompatible with human macrophages, making them promising drug candidates for further investigations in this field.

Synthesis and Characterization of New Heterocyclic Compounds from 2, 5- dimercapto -1, 3, 4-Thiadiazole and Their Resins

In this research, a new 1, 3, 4-Thiadiazole derivatives have been synthesized by many heterocyclic reactions. Starting from (2, 5 – dimercapto -1, 3, 4-Thiadiazole) a variety of derivatives have been synthesis. Compound (1) was synthesized by the reaction of hydrazine hydrate with carbon disulphide in absolute ethanol. The compound (1) was reacted with 1, 2-dibromoethane in presence of alkali ethanol to give the compound (2). The compound (3) was formed from the reaction of compound (2) with hydrazine hydrate. Schiff base (4) was obtained by reacting of compound (3) with the compound (p-hydroxybenzaldehyde) in absolute ethanol. A variety of phenolic Schiff base (Methylolic, Etheric, and Epoxy) derivatives have been synthesized. Methylolic derivative was synthesized by the reaction of Schiff base (4) with formaldehyde in tetrahydrofuran (THF). Etheric derivative was formed from the reaction of a methylolic Schiff base (5) with saturated alcohol (Methanol).Epoxy derivative was synthesized by the reaction of epichlorohydrine with etheric derivative (6) .The last step of this research was the preparation of a composite material from mixing the Epoxy resin derivative(7), TiO2and morpholine via ring opening. All these derivatives were verified by using (FT-IR, UV) spectra photometer and 1H-NMR spectra. Also, these derivatives were characterized using elemental analysis (C.H.N.S) .

Novel Triazine Schiff Base-Based Cationic Gemini Surfactants: Synthesis and Their Evaluation as Antiwear, Antifriction, and Anticorrosive Additives in Polyol

Two novel triazine Schiff base-based cationic gemini surfactants namely N,N′-bis{(p-(N,N,N-tetradecyldimethylammonium bromide)benzylidene} 6-methyl-1,3,5-triazine-2,4-diamine (14-MTR-14) and N,N′-bis{(p-(N,N,N-tetradecyldimethylammonium bromide)benzylidene} 6-phenyl-1,3,5-triazine-2,4-diamine (14-PTR-14) were synthesized following the two-step reaction. First the intermediate adduct was synthesized by reaction of the 4-(dimethylamino)benzaldehyde with 1-bromotetradecane. In the second step, the germinal surfactants 14-MTR-14 and 14-PTR-14 were synthesized by imine coupling with this intermediate adduct with 6-methyl-1,3,5-triazine-2,4-diamine and 6-phenyl-1,3,5-triazine-2,4-diamine, respectively. Both were characterized using elemental analysis (CHN), infrared (IR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, and thermogravimetry (TG). The compounds were then evaluated as anticorrosive and lubricity improver additive in polyol lube base oil. Both the surfactants show the similar anticorros...

Synthesis, characterization, in vitro cytotoxicity, in silico ADMET analysis and interaction studies of 5-dithiocarbamato-1,3,4-thiadiazole-2-thiol and its zinc(ii) complex with human serum albumin: combined spectroscopy and molecular docking investigations

The binding site of new complex Zn(ii) of 5-dithiocarbamato-1,3,4-thiadiazole-2-thiol and HAS.

Synthesis and Characterization of New Heterocyclic Compounds from 2, 5- dimercapto -1, 3, 4-Thiadiazole and Their Resins

In this research, a new 1, 3, 4-Thiadiazole derivatives have been synthesized by many heterocyclic reactions. Starting from (2, 5 – dimercapto -1, 3, 4-Thiadiazole) a variety of derivatives have been synthesis. Compound (1) was synthesized by the reaction of hydrazine hydrate with carbon disulphide in absolute ethanol. The compound (1) was reacted with 1, 2-dibromoethane in presence of alkali ethanol to give the compound (2). The compound (3) was formed from the reaction of compound (2) with hydrazine hydrate. Schiff base (4) was obtained by reacting of compound (3) with the compound (p-hydroxybenzaldehyde) in absolute ethanol. A variety of phenolic Schiff base (Methylolic, Etheric, and Epoxy) derivatives have been synthesized. Methylolic derivative was synthesized by the reaction of Schiff base (4) with formaldehyde in tetrahydrofuran (THF). Etheric derivative was formed from the reaction of a methylolic Schiff base (5) with saturated alcohol (Methanol).Epoxy derivative was synthesized by the reaction of epichlorohydrine with etheric derivative (6) .The last step of this research was the preparation of a composite material from mixing the Epoxy resin derivative(7), TiO2and morpholine via ring opening. All these derivatives were verified by using (FT-IR, UV) spectra photometer and 1H-NMR spectra. Also, these derivatives were characterized using elemental analysis (C.H.N.S) .

Synthesis and spectroscopic characterization of Zn(II), Cd(II), and Hg(II) ciprofloxacin complexes

Ciprofloxacin metal co mplexes with general for mula [M(CPF)2]X2·nH2O [M = Zn(II), Cd(II), and Hg(II)] have been synthesised and characterized using elemental analysis (CHN), spectroscopic (UV-Vis, IR, MS, and 1H NMR) and ther mogravimetric (TG and DTA) data. Using the Coats-Redfern and Horowitz-Metzeger methods, kinetic analysis of the thermogravimetric data had been performed.

Synthesis, spectroscopic and thermal characterization of sulpiride complexes of iron, manganese, copper, cobalt, nickel, and zinc salts. Antibacterial and antifungal activity

Sulpiride (SPR; L) is a substituted benzamide antipsychotic which is reported to be a selective antagonist of central dopamine receptors and claimed to have mood-elevating properties. The ligation behaviour of SPR drug is studied in order to give an idea about its potentiality towards some transition metals in vitro systems. Metal complexes of SPR have been synthesized by reaction with different metal chlorides. The metal complexes of SPR with the formula [MCl(2)(L)(2)(H(2)O)(2)].nH(2)O [M=Mn(II), Co(II), Ni(II), Cu(II) and Zn(II); n=0-2] and [FeCl(2)(HL)(H(2)O)(3)]Cl.H(2)O have been synthesized and characterized using elemental analysis (CHN), electronic (infrared, solid reflectance and (1)H NMR spectra) and thermal analyses (TG and DTA). The molar conductance data reveal that the bivalent metal chelates are non-electrolytes while Fe(III) complex is 1:1 electrolyte. IR spectra show that SPR is coordinated to the metal ions in a neutral monodentate manner with the amide O. From the magnetic and solid reflectance spectra, octahedral geometry is suggested. The thermal decomposition processes of these complexes were discussed. The correlation coefficient, the activation energies, E*, the pre-exponential factor, A, and the entropies, DeltaS*, enthalpies, DeltaH*, Gibbs free energies, DeltaG*, of the thermal decomposition reactions have been derived from thermogravimetric (TG) and differential thermogravimetric (DTG) curves. The synthesized ligand and its metal complexes were also screened for their antibacterial and antifungal activity against bacterial species (Escherichia coli and Staphylococcus aureus) and fungi (Aspergillus flavus and Candida albicans). The activity data show that the metal complexes are found to have antibacterial and antifungal activity than the parent drug and less than the standard.