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.
The cost-effective removal of heavy metal ions represents a significant challenge in environmental science. In this study, we developed a straightforward and efficient reusable adsorbent by amalgamating chitosan and vermiculite (forming the CSVT composite), and comprehensively investigated its selective adsorption mechanism. Different techniques, such as Fourier-transform infrared spectroscopy (FTIR), zeta potential analysis, scanning electron microscopy (SEM), X-ray diffraction (XRD), and Brunauer, Emmett, Teller (BET) analysis were employed for this purpose. The prepared CSVT composite exhibited a larger surface area and higher mesoporosity increasing from 1.9 to 17.24 m2/g compared to pristine chitosan. The adsorption capabilities of the
... Show MoreSchiff bases, named after Hugo Schiff, are aldehyde- or ketone-like compounds in which the carbonyl group is replaced by imine or azomethine group. They are widely used for industrial purposes and also have a broad range of applications as antioxidants. An overview of antioxidant applications of Schiff bases and their complexes is discussed in this review. A brief history of the synthesis and reactivity of Schiff bases and their complexes is presented. Factors of antioxidants are illustrated and discussed. Copyright © 2016 John Wiley & Sons, Ltd.
The synthesis of ligands with N2S2 donor sets that include imine, an amide, thioether, thiolate moieties and their metal complexes were achieved. The new Schiff-base ligands; N-(2-((2,4-diphenyl-3-azabicyclo[3.3.1]nonan-9-ylidene)amino)ethyl)-2-((2-mercaptoethyl)thio)-acetamide (H2L1) and N-(2-((2,4-di-p-tolyl-3-azabicyclo[3.3.1]nonan-9-ylidene)amino)ethyl)-2-((2-mercaptoethyl)thio) acetamide (H2L2) were obtained from the reaction of amine precursors with 1,4-dithian-2-one in the presence of triethylamine as a base in the CHCl3 medium. Complexes of the general formula K2<
New metal complexes of the ligand 4-[5-(2-hydoxy-phenyl)-[1,3,4- oxadiazol -2-ylimino methyl]-1,5-dimethyl-2-phenyl-1,2-dihydro-pyrazol-3-one (L) with the metal ions Co(II), Ni(II), Cu(II) and Zn(II) were prepared in alcoholic medium. The Schiff base was synthesized through condensate of [4-antipyrincarboxaldehyde] with[2-amino-5-(2-hydroxy-phenyl-1,3,4- oxadiazol] in alcoholic medium . Two tetradentate Schiff base ligand were used for complexation upon two metal ions of Co2+, Ni2+, Cu2+ and Zn2+ as dineucler formula M2L2.4H2O. The metal complexes were characterized by FTIR Spectroscopy, electronic Spectroscopy, elemental analysis, magnetic susceptidbility measurements, and also the ligand was characterized by 1H-NMR spectra, and m
... Show MoreThe work includes synthesis of 1,2,3-triazoles via click conditions and using the microwave irradiation starting from two synthesized azides: 2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl azide (5) and perfluorobutylethyl azide (10) and different terminal alkynes. It also includes microwave enhanced synthesis of tetrazoles via the reaction of two synthesized azides i.e., perfluorobutylethyl azide (10) and 1,5-diazidopentane (13) with benzoyl cyanide. Most of the prepared compounds have been characterized by: TLC, FT-IR, 1H NMR, 13C NMR, LC-MS and microelemental analysis
.Curcumin (Cur) and L phenylalanine (Phy) compounds were used to prepare two mixed ligand complexes with Cr (III) and Fe (III) ions. The synthesized complexes are characterized by using conductivity measurement and different spectral methods like FT-IR and UV- Vis .Molar conductance and analytical studies confirmed that the complexes exhibit octahedral geometry., suggest that the complexes are formed in 1: 1 :2 [ L : Metal : 2phe ] ratio and they proposed to have the general formulae [M(Cur)(phe)2] Cl (M= Cr (III) and Fe (III) The compound dyeing method was studied and applied to acrylic fabric.The antibacterial activity of curcumin, phenylalanine and their mixed ligand complexes were examined on pathogenic bacterial strains and showed good
... Show MoreNon-steroidal anti-inflammatory drugs (NSAIDs) contain free –COOH which thought to be responsible for the GI irritation associated with all traditional NSAIDs. The esterification of this group is one of an approach to ultimate aim for reduce the gastric irritation; so in this study we synthesized and preliminarily evaluated new ester compounds as new analogues with expected selectivity toward COX-2 enzyme. Synthetic procedures have been successfully developed for the generation of the target compounds (III a and b). The synthetic approach involved multi-steps procedures which include: Synthesis of 4-hydroxy benzene sulphonamide ( I b ), synthesis of Naproxen and Ibuprofen acyl chloride and then reacting them with 4-hydroxy benzene sulphon
... Show MoreSoil that has been contaminated by heavy metals is a serious environmental problem. A different approach for forecasting a variety of soil physical parameters is reflected spectroscopy is a low-cost, quick, and repeatable analytical method. The objectives of this paper are to predict heavy metal (Ti, Cr, Sr, Fe, Zn, Cu and Pb) soil contamination in central and southern Iraq using spectroscopy data. An XRF was used to quantify the levels of heavy metals in a total of 53 soil samples from Baghdad and ThiQar, and a spectrogram was used to examine how well spectral data might predict the presence of heavy metals metals. The partial least squares regression PLSR models performed well in pr