The purpose of my thesis is to prepare four new ligands (L1-L4) that have been used to prepare a series of metal complexes by reacting them with metal ions: M=(Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II) Where succinyl chloride was used as a raw material for the preparation of bi-dented ligands (L1-L4) by reacting it with potassium thiocyanate as a first step and then reacting with (2-aminobenzothiazole, Benzylamine, 4-aminoantipyrine, Sulfamethoxazole) respectively as a second step with the use of dry acetone as a solvent, the chemical formula of the four ligands prepared in succession: N1,N4-bis(benzo[d]thiazol-2-ylcarbamothioyl)succinamide (L1) N1,N4-bis(benzylcarbamothioyl)succinamide (L2) N1,N4-bis((1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl) carbamothioyl)succinamide (L3) N1,N4-bis((4-(N-(5-methylisoxazol-3-yl)sulfamoyl) phenyl) carbamo thioyl) succinamide (L4) The new ligands were identified using spectroscopic measurements that included (FT-IR spectra, UV-Vis spectra, and nuclear magnetic resonance (1H, 13CNMR) spectra, mass spectra, elemental analysis (C.H.N.S), and thermal analysis (TGA&DSC), as the results of the measurements proved to be identical to the proposed molecular formula for these ligands. A series of metal complexes for ligands was also prepared, which included seven complexes for each ligand, by adding each of the metal ions to the four ligands prepared in succession to produce the following molecular formulas: - [M2(L)Cl4] , L= L1, L2, L3, L4 (M= Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II)) The prepared complexes were diagnosed by several techniques, including the study of the infrared spectra of the prepared complexes, and when comparing those spectra with the spectra of each of the four ligands prepared in the free form, these gave clear changes, including the emergence of a new band within the fingerprint area. It was not originally present in the spectra of ligands in their free form, and this is due to the occurrence of coordination between the metal ions under study and the donor atoms, which are the oxygen atom of the (C=O) group, and the sulfur atom of the (C=S) group in the ligands. (L1-L4), while other distinct bands were obtained with clear changes in shape, intensity, and location, and this is an indication of the occurrence of a coordination process between the metal ions under study and the four prepared ligands. The percentage of metal ions in the prepared complexes was determined by flame atomic absorption spectrometry, where it was shown from the careful analysis of the elements the great agreement between the percentages calculated theoretically and obtained practically. The magnetic sensitivity results showed that some of the prepared metallic complexes have paramagnetic properties. The measurements of the molar conductivity of the prepared complexes dissolved in DMSO at a concentration of 1×10-3 M and at the laboratory temperature showed that they are of a non-electrolytic nature. The prepared complexes were also studied through solubility, melting point, and ultraviolet-visible techniques, and through the data of all the aforementioned techniques, structural formulas were proposed for the prepared complexes, through which it was found that the prepared ligands are bivalve chelating ligands that lead to their participation as ligand into complexes with a tetrahedral geometric shape for all metallic complexes under study. The research included a study evaluating the antioxidant activity of some selected metal complexes by studying the amount of radical scavenging of DPPH* compared to ascorbic acid as an antioxidant reference agent. The zinc complex showed higher activity than the nickel complex compared to standard ascorbic acid. The [Cu2(L1)Cl4] and [Co2(L1)Cl4] complexes were also tested as antibodies to inhibit the breast cancer cell line (MCF-7) and compared with the normal cell line (HdFn), where the copper complex showed the ability to inhibit the cancerous cell line compared with the cobalt complex. The molecular binding of ligands (L3) and (L4) was also studied, and their possibility of using them as drugs in the treatment of some diseases, where the ligand L3 showed better association with the active site of the enzyme than the ligand L4, and is expected to highest antimicrobial effect. Finally, the biological effect of the prepared ligands and some of their complexes on the growth of two types of bacteria, Escherichia coli and Staphylococcus aureus, was studied using DMSO solvent, where the complexes showed greater activity than the ligands against the selected types of bacteria.
Schiff base (methyl 6-(2- (4-hydroxyphenyl) -2- (1-phenyl ethyl ideneamino) acetamido) -3, 3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0] heptane-2-carboxylate)Co(II), Ni(II), Cu (II), Zn (II), and Hg(II)] ions were employed to make certain complexes. Metal analysis M percent, elemental chemical analysis (C.H.N.S), and other standard physico-chemical methods were used. Magnetic susceptibility, conductometric measurements, FT-IR and UV-visible Spectra were used to identified. Theoretical treatment of the generated complexes in the gas phase was performed using the (hyperchem-8.07) program for molecular mechanics and semi-empirical computations. The (PM3) approach was used to determine the heat of formation (ΔH˚f), binding energy (ΔEb), an
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AS Muhsen, International Journal of Psychosocial Rehabilitation (1475-7192), 2020 - Cited by 1
This research includes the synthesis of some new different heterocyclic derivatives of 5-Bromoisatin. New sulfonylamide, diazine, oxazole, thiazole and 1,2,3-triazole derivatives of 5-Bromoisatin have been synthesized. The synthesis process started by the reaction of 5-Bromoisatin with different reagents to obtain schiff bases of 5-Bromoisatin intermediate compounds(1, 8, 19) by using glacial acetic acid as a catalyst in three routes. The first route, 5-Bromoisatin reacted with p-aminosulfonylchloride to product compound(1), then converted to sulfonyl amide derivatives(2-7) by the reaction of compound(1) with different substituted primary aromatic amine in absolute ethanol. The second route includes the reaction of 5-Bromoisatin rea
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Methotrexate (MTX) is one of the most effective medications to treat rheumatoid arthritis (RA).Aserum of 60 Iraqi male patients suffering from RA as (G1) was newly diagnosis and the same patient in G1 after taking MTX as G2 and 40 Iraqi male healthy control as G3. Nesfatin-1 (Nf-1) is belong to the adipokine family withpleiotropic effect. Nf-1 has been found in different tissues, including stomach, pancreas, bone cells, cartilage and heart. Retinol binding protein (RBP4) was known as transpoter of retinol from its storage sites in the liver to the extrahepatic tissues. Moreover, RBP4 acts as adipokine and contributes in the pathophsyology of prototypic inflammatory disease, rheumatoid arthritis (RA). The results showed a significant increas
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Worldwide attention is being focused on nanocrystalline zeolites and they are replacing conventional ones due to their pronounced potential in many fields. In this study, NaY zeolite has been prepared hydrothermally using sol –gel method and modified to the proton type by ion –exchange process. Characterization is made using X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), Atomic force microscopy (AFM), Brunauer –Emmet- Teller (BET) nitrogen adsorption method, Ammonia Temperature programmed desorption (NH3-TPD) and Scanning electron microscopy( SEM). The effect of aging time, silica to alumina ratio is studied and the results sh
... Show MoreThe reaction of(2-oxo-2H-chromen-3-Carbonyl chloride)(k1) with hydrazine in boiling ethanol gives the hydrazide(K2).When compound (k2) reacts with various aromatic aldehydes ,the corres ponding Schiff bases(k3–k4) achieve new series of thiazotidines (k5–k6) and azetidinones (k7–k8) obtained from the reactions of appropriate Schiff bases with mercapto acetic acid and chloro acetyl chloride respectively. All the compounds are characterized by FT-IR,1H-NMR and GC-Ms.
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The polyaniline powder was chemically manufactured by direct oxidation of aniline. The resulting polymer was characterized by the results of optical, measurements by (FT-IR) spectroscopy, we have detected some of the absorption peaks located at 3498, 2858 cm-1, which correspond N-H vibrations, and C-H expansion of the aromatic ring respectively as well as stretching vibrations of quinoid ring have been observed. Structural properties, such as the surface topography using an atomic force microscope (AFM), and Surface composition by (SEM) have been studied. The structure of some pellets of polyaniline powder have been examined by using analytical X-ray diffraction technique, the pattern of obse
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Derivatives of Schiff-bases possess a great importance in pharmaceutical chemistry. They can be used for synthesizing different types of bioactive compounds. In this paper, derivatives of new Schiff bases have been synthesized from several serial steps. The acid (I) was synthesized from the reaction of dichloroethanoic acid with 2 moles of p-aminoacetanilide. New acid (I) converted to its ester (II) via the reaction of (I) with dimethyl sulphate in the present of anhydrous of sodium carbonate and dry acetone. Acid hydrazide (III) has been synthesized by adding 80% of hydrazine hydrate to the new ester using ethanol as a solvent. The last step included the preparation of new Schiff-bases (IV-VIII) by the reaction of acid hydrazide with app
... Show MoreDerivatives of Schiff-bases possess a great importance in pharmaceutical chemistry. They can be used for synthesizing different types of bioactive compounds. In this paper, derivatives of new Schiff bases have been synthesized from several serial steps. The acid (I) was synthesized from the reaction of dichloroethanoic acid with 2 moles of p-aminoacetanilide. New acid (I) converted to its ester (II) via the reaction of (I) with dimethyl sulphate in the present of anhydrous of sodium carbonate and dry acetone. Acid hydrazide (III) has been synthesized by adding 80% of hydrazine hydrate to the new ester using ethanol as a solvent. The last step included the preparation of new Schiff-bases (IV-VIII) by the reaction of acid hydrazide with
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The reaction of some new Schiff bases ( 2-[(2-Amino – ethylimino)-methyl]-R , 2-({2-[(R-benzylidene)-amino]-ethylimino}-methyl)-R with Benzoyl chloride or Acetyl chloride were carried out. Subsequent reactions of these products N-(2-Amino-ethyl)-N-[Chloro-(R) –methyl]-benzamide or N-(2-{?-[chloro-(R) –methyl]-amino}-ethyl)-N-[chloro-(R) –methyl]- benzamide with thiourea afforded thioureas compounds. The synthesized compounds were confirmed by their IR,UV,spectra and C.H.N. analysis.