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تخليق مشتقات جديدة لمركبات اللاكتام و البريميدين و دراسة فعاليتها كمضادات للاكسدة و مضادات للاورام Synthesis, Anti - Oxidant And Anti - Tumor Activity Of New Lactam And Pyrimidine Derivatives

المستخلص: In the end of last century the increasing of cancer disease has been speared in worldwide, has been pushing to investigate more in synthesis a new drug treatment herein, the idea in this thesis three types of heterocyclic compounds | were synthesized : | 1- Synthesis of a series of β-lactams 3(a-h) compounds by using Kinugasa reaction and Staudinger reaction, which β-lactam 3(a-b) compounds (as depicted in scheme below) were synthesized using Kinugasa reaction by reacting alkyne (phenylacetylene and 1-octyne) with the appropriate nitrones 2(a-b) in the presence triethylamine and CuI as catalyst and acetronitrel as solvent at 0˚C. R1 : 4-NHCOCH3 , 3-NO2 R2 : CH3(CH2) , 5 While β-lactam 3(c-h) compounds (as depicted in scheme below) were synthesized using Staudinger reaction by reacting methoxyacetyl chloride with the appropriate imines 2(c-h), in the presence of triethylamine in dry dichloromethane under nitrogen atmosphere at 0˚C.3c : R1= −C6H4Cl , R2= −C6H4− , 3f : R1= −C6H4Me , R2= −C6H4− | 3d : R1= −C6H4Br , R2= −C6H4− , 3g : R1= −C6H4Br , R2= −C6H4− 3e : R1= −C6H4Cl , R2= −C6H4− , 3h : R1= −C4H4N2 , R2= −C6H4− 2- Synthesis of a series of γ-lactams 4(a-h) (as depicted in scheme below) by reaction phenylsuccinic anhydride or 3-(4-chlorophenyl)dihydrofuran-2,5- dione with schiff bases (imines) 2(d,e,g,i,j,k,l,m), by using chloroform as solvent and heated at temperature (55-60˚C) Synthesis of a series of 3,4-Dihydropyrimidin-2(1H)-ones/ thiones 5(a-g) (as | depicted in scheme below) by reaction aldehyde, ethyl acetoacetate and | urea/thiourea under FeCl3.6H2O as catalyst, by using ethanol as solvent and heated at reflux temperature. | H2N NH2 | FeCl3.6H2O | ethanol , reflux | ethyl acetoacetate urea or thiourea aldehyde 5(a-g)The final products were characterized by using the basis of the spectral data : | IR, 1H-NMR, 13C-NMR and Mass. | The antioxidant activity for the synthesized compounds (3g, 4a, 5a) were examined and show highly biological activity response. Moreover, the activity against breast cancer MCF-7 cell line also studied and exhibited highly anti tumor.
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: دكتوراه
الموضوع الدقيق: الكيمياء العضوية
السنة: 2018
الموضوع العام: علوم الكيمياء
اسم المشرف: محمود شاكر مكطوف التميمي حسام محمد كريديا
اسم المؤلف: عبد الرحمن يسر خليفة الغزي

تقدير بعض العناصر الثقيلة في نماذج حقيقية باستعمال مركبات ازو - ازوميثين جديدة بواسطة استخلاص نقطة الغيمة Determination Of Some Heavy Metals In Real Samples Using New Azo - Azomethine Compounds By CPE

المستخلص: Since its inception in 1985, Cloud-point extraction (CPE) methodology has constituted an important theme in the analytical chemistry as promising procedure for the separation and preconcentration for the metal ions and organic compounds from the complex matrices samples. Nowadays, it has been begins to take a large noteworthy position among the other modern separation methods in scientific research and application on a high level due to its simplicity, rapidity, more precise and cheapness beside an environmentally-friendly method, therefore, this research includes three main chapters . | Chapter One includes introduction of azo-azomethine compounds and their complexes and a view of the different extraction techniques, fundamental principles and potential applications of CPE methodology in analytical chemistry. It also involves a concise review on the latest developments of the method and its applications for the determination of cadmium, copper and cobalt by CPE . | Chapter Two consists of an outline of different instrumental techniques , general apparatus and chemicals used in the present work. | The synthesis paths of azo-azomethine compounds (L1 to L4) and primary testing of complex formation between metal ions and reagents, determination of λmax . As well as optimization of the experimental conditions (volume reagent, reaction time, temperature and pH) and determination of dissociation degree and stability constant, stoichiometry of the complex (Continuous variation method -Job method). In addition CoCl2.6H2O and L4 with salts CrCl3.6HO and CdCl2.H2O. The analytical | procedures for CPE which were designed for the determination of analytes including optimization of the Parameters for CPE including (reagent concentration, HCl concentration, incubation time, equilibration temperature, thermodynamic study and Triton X-100 volume) were selected in this study. The present CPE method was applied for determination concentration of metal ions (Cd2+, Cu2+ and Co2+) in real samples by FAAS. | Chapter Three included the new azo-azomethine compounds prepared and their complexes which were characterized by various analytical techniques as a UV-Visible spectroscopy(UV-Vis), Infrared Spectroscopy(FT-IR), Nuclear Magnetic Resonance Spectroscopy(1HNMR), Mass Spectra and Molar Electrical Conductivity for complexes and the results were identical to what is expected scientifically. The spatial shape of the complexes which was prepared is (octahedral) and stoichiometry of the complex. It’s ratio 1 : 1. | In chapter three, there are too highlights on the results and discussion in analytical applications for the separation and preconcentration for the metal with separation and extraction method, such as cloud-point extraction (CPE) as an separation technique that uses a surfactant, instead of organic solvents for phase separation. | In the first part of CPE, Analytical reagent namely 6-((1E)-((2-(((E)-2-hydroxy-3-methoxy-4-((6-methoxybenzo[d]thiazol-2- yl)diaz enyl)benzylidene)amino)benzyl)imino)methyl)-2-methoxy-3- ((6- methoxybenzo[d]thiazol-2-yl)diazenyl)phenol (L1) after synthesis and characterization by using various analytical techniques as a preliminary using various analytical techniques as a preliminary step toward its using | as an organic reagent for the formation of an ion-association complex | with copper ion in acidic medium, apt to interact with surfactant in | solution. The L2 as a reagent for the formation of an ion association | complex with copper in acidic solution and the complex is extracted into | the surfactant Triton X-100 at optimum conditions. The surfactant-rich | phase which contains copper complex is mediated with solvent and the | Cu content measured by FAAS (λmax = 324.75 nm) . The effects of the several variables which affect the CPE efficiency are optimized by OFAT procedure beside other parameters with which one is mentioned with Cu(II) . The thermodynamic study was also investigated to expand the understanding of the mechanism of solvation of Cu(II) in the micelles . | Under the optimized condition established, the enrichment factor of 52.574 was achieved for Cu2+ with the L2 . The concentration range of (0.01-3) μg ml-1 leads to detection limit of 0.017238 μg ml-1. The precision for ((%RSD, n=8) at 0.05μg.ml-1 Cu2+ was of %1.063. The developed method was used for the determination concentration of Cu2+ in real samples. The accuracy was determined by recovery percentage for real samples, it’s found good recoveries (100.380-103.377%) for Cu2+ with L2. | In the third part CPE, Analytical reagent namely6-(((2-(((E)-2- hydroxy-3-methoxy-4-(o-tolyldiazenyl)benzylidene)amino) benzyl)imino)methyl)-2-methoxy-3-(o-tolyldiazenyl)phenol(L3)was synthesised and fully characterized by using various analytical techniques | as a preliminary step toward its using as an organic reagent for the formation of an ion-association complex with cobalt ion in acidic medium and the complex is extracted into the surfactant Triton X-100 at optimum conditions for determination of Co(II) as CoCl4 | 2- ion by using the combined cloud point extraction (CPE) methodology. After phas separation, the surfactant-rich phase was diluted with 1M HNO3 in methanol and cobalt (II) ion determined by FAAS technique at λmax of 240.72 nm. The optimization of complexation and extraction conditions was investigated. Thermodynamic parameters of CPE for solubilization process of the ion-pair complex in Triton X-100 were also considered. | Under the optimized conditions, the preconcentration of a 15ml sample which gave preconcentration and enrichment factors were of 15 and 54.078 respectively. The calibration graph was linear in the range of (0.025-3) μg ml-1 with a limit of detection and quantitation limit 0.011534 and 0.038446 μg ml−1. The relative standard deviation for replicate determinations at 0.05μg ml−1 level was of (0.823%, n=8). The proposed | method was applied for the determination of cobalt in river, tap waters, milk, black tea , tobacco and soil by FAAS. The accuracy was determined by recovery percentage for real samples, it’s found good recoveries (101.108-104.918%) for Co2+ with L3 . The study of the stoichiometry for ion association complexes using the slope analysis technique showed that the ion association complex ratio was 1 : 1 for all extracted complexes
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: دكتوراه
السنة: 2018
الموضوع العام: علوم الكيمياء
اسم المشرف: ساهر عبد الرضا علي الشمخاوي
اسم المؤلف: ساجدة صبار عفات

دراسات سريرية وجينية في امصال الدم والسائل المنوي للمدخنين وغير المدخنين المصابين بالعقم غير المفسر في محافظة ذي قار - العراق Biochemical and Genetic Studies of Sera and Semen for Smokers and Non Smokers with Unexplained Male Infertility in Thi - Qar Province/ Iraq

المستخلص: This study was conducted on infertile subjects attending to the infertility Unit in Al-Hussein Teaching Hospital in Thi-Qar province south of Iraq, during the period from Aug 2016 to May 2017. The aim of study was to determine the roles of the presence of some biochemical parameters (oxidative stress, antioxidants), antisperm antibodies and polymorphism for glutathione peroxidase (GPx1) and glutathione transferase (GTSp1) in men with unexplained infertility. | Ninety men with unexplained male infertility (UMI) aged (91-91) year and fifty healthy fertile men aged (20-25) year were included in this study as a control group, had no systemic diseases and none were taking an oral antioxidant supplement for three months prior to the study. | The patients and control were divided into two groups (smoker and non smoker). Serum and seminal fluids were collected from each of them, seminogram test (semen analysis) was performed for each participant, and all semen samples were collected following (3-5) days of abstinence. After liquefaction, semen volume, sperm concentration, total sperm count, morphology, motility grades were determined using World Health Organization (WHO) standard procedures. | In this study, there is no significant (P>0.05) between age and body mass index (BMI) of unexplained infertile men compared with age of fertile men (control). The groups of the unexplained infertile males with history of infertility of 3-5 years duration were largest groups who attended medical services. The majority of the unexplained infertile men (90%) complained of primary infertility while the minority of them (10%) complained of secondary infertility. The current study revealed that effect smoking on unexplained infertile group was percentage (44.4%) comparison with control fertile group (36 %). | )II( | The results of semen analysis for the fertile (control) and the unexplained infertile men, revealed no significant differences (P>0.05) in semen volume, liquefaction time, and semen pH between the two groups in (smoker and non smoker). A significant decrease (P<0.05) was seen in the sperm concentration, sperm motility, total progressive sperm (progressive sperm motility and non-progressive sperm motility) and normal sperm morphology in the unexplained infertile group compared with the fertile group (control). While a significant increase (P<0.05) was seen in immotile sperm, sperm agglutination, round cells count and leukocytes in the unexplained infertile group compared with the fertile group (control). | The results showed a significant increase (P<0.05) in serum and seminal plasma Malondialdehyde (MDA) in unexplained infertile (smoker and nonsmoker) groups when compared to fertile (smoker and nonsmoker) groups. The antioxidant such as vitamins (C and E) and glutathione were significantly decreased in serum and seminal plasma for unexplained infertile (smoker and nonsmoker) groups when compared to fertile (smoker and nonsmoker) groups. | A significant increase in serum Ceruloplasmin(Cp) levels in unexplained infertile group comparison with fertile (control) group (P<0.05). Significant differences (P<0.05) in seminal plasma fertile (smoker and non smoker) groups but there was no statistical difference in the Ceruloplasmin level of seminal plasma unexplained infertile between two groups (smoker and non smoker) groups and no significant difference between smoker fertile group with unexplained Infertile (smoker and non smoker) groups. | High prevalence of antisperm antibody (ASA) in seminal plasma for unexplained male infertility a percentage (25.5%) compared with infertility (control) a percentage (14%), and significant differences in ASA seminal plasma | )III( | (Smoker and non smoker) in all groups, which indicator that high in Smoker men compared with non smoker . | In this research found association between the glutathione peroxidase (GPx1) polymorphism and unexplained male infertility, and effect oxidation and antioxidant on these. Therefore, might be a major risk factor of unexplained male infertility in the studied groups, suggested a stronger association between smoking consumption and risk of unexplained male infertility. | The frequency of the glutathione transferase (GSTp1) genotype showed almost no difference between the unexplained infertile men and the fertile controls, therefore, in this case-control study, the GSTp1 variant genotype (Ile/ Ile ,Ile/ Val , Val/ Val) was no significant different in every group of unexplained infertile men compare than in the fertile (control group).This indicating no significant association between GSTp1 and sperm parameters.
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: دكتوراه
السنة: 2019
الموضوع العام: علوم الكيمياء
اسم المشرف: رائد معلك حنون ساجد حسن كزار
اسم المؤلف: وسام ريسان نايف المحسن

دراسة وظائف الكبد وصورة الدهون والاجهاد التاكسدي في مصول النساء قبل وبعد استئصال المرارة في محافظة ذي قار / العراق Study of Liver Function, Lipid Profile and Oxidative Stress in Sera of Women Pre and Post Cholecystectomy in Province of Thi - Qar/ Iraq

المستخلص: The present study has been designed to evaluate and compare changes in patients pre, post and long periods for cholecystectomy on BMI, liver function (Aspartate Amino Transferase (AST), Alanine Amino Transferase (ALT), Alkaline Phosphatase (ALP), Total Bilirubin (TSB), Total Protein (TP), lipid profile (Total Cholesterol (TC), Triglyceride (TG), High Density Lipoprotein (HDL), Low Density Lipoprotein (LDL), Very Low Density Lipoprotein (VLDL)), oxidative stress (Malondialdehyde (MDA), Nitric Oxide (NO)) and antioxidant state (Albumin (Alb), Ceruloplasmin (CP)). | The study includes (192) subjects : (64) normal subjects (control) and (128) patient’s cholecystectomy, their age range (20-69) years, the patients were divided in to three groups : (64) patients pre and 24 hr post operation cholecystectomy, (64) patients after long periods for cholecystectomy, as well as the patients were divided by age into two groups : a premenopausal group and a postmenopausal group. | The results show that there were a significant decreased in the concentration of serum (AST, ALT, TSB, DB, InB, HDL and Alb) in group pre in comparison with each of post (short and long terms) and control groups (p≤0.05). It was found no significant differences in the concentration of serum (AST, ALT, TSB, DB, InB, HDL and Alb) between each of post (short and long terms) groups (p≤0.05). Also it was found significant differences in the concentration of serum (AST, ALT, TSB, DB, InB, HDL and Alb) between each of post (short and long terms) and control groups (p≤0.05). | -----------------------------INDEX--------------------------------- | XII | While the results showed a significant increase in the concentration of serum (ALP, TP, TC, LDL, NO, MDA and Cp) in all patient groups in comparison with control groups (p≤0.05). It was found no significant differences in the concentration of serum (ALP, TP, TC, LDL, NO, MDA and Cp) between each of post (short and long terms) groups (p≤0.05). Also it was found significant differences in the concentration of serum (ALP, TP, TC, LDL, NO, MDA and Cp) between each of post (short and long terms) and control groups (p≤0.05). | Also the results showed a significant increase in the concentration of serum TG and VLDL in all patient groups in comparison with control groups (p≤0.05). It was found no significant differences in the concentration of serum TG and VLDL between each of post (short and long terms) groups in the group A (p≤0.05). But it was found a significant difference in the concentration of serum TG and VLDL between each of post (short and long terms) in the group B (p≤0.05). Also it was found a significant difference in the concentration of serum TG and VLDL between each of post (short and long terms) groups and control groups (p≤0.05). | The correlation between nitric oxide and each of (ALP, TP, TC, TG, LDL, VLDL, MDA and Cp) in these patient groups were positive. Whereas the correlation between nitric oxide and each of (AST, ALT, TSB, BD, InB, HDL and Alb) in these patient groups were negative. | The above reviewed results lead to conclusion that cholecystectomy causes variant alternations in serum hepatic function and lipid profiles and causes variant effects in serum oxidative stress. Also, age has no effect on each of (ALT, TSB, DB, InB, ALP, TP, TG, VLDL, NO, MDA, Cp and Alb), while age has effect on each of (TC, LDL and HDL). Besides, there are no effect of the period after cholecystectomy on all studied parameters except TG and VLDL.
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: ماجستير
السنة: 2018
الموضوع العام: علوم الكيمياء
اسم المشرف: رائد معلك الصالح مهند عبد الرضا الشريفي
اسم المؤلف: سمى يعقوب يوسف

تحوير فجوة طاقة ثاني اوكسيد التيتانيوم بواسطة تفاعلات الحالة الصلبة مع صوديوم بوروهيدريد والمنيوم ليثيوم هيدريد وتحديد فعالية التحفيز الضوئي Modifying The Band Gap of Nano Titanium Dioxide By Solid State Reactions With Aluminum Lithium Hydride and Sodium Borohydride and Determining Their Photocatalytic Activity

المستخلص: This study includes preparation of nanoparticles of titanium dioxide using sol-gel method and then, the band gap was modified by solid state reaction with (AlLiH4،NaBH4) reductive compounds. Modification reduced the band gap separating | energy levels between valance band (VB) and conduction band (CB), therefor; facilitating the transfer of excited electrons from (VB) to (CB). Absorption of the energy from incident photons having the same or larger energy than the energy of the | band gap promote the formation of the couple (electron - hole) . The resulting (e--h+) couple acts to produce (OH.) radicals. OH. radicals hav a high capability to destroy organic pollutants that adsorbed on surface of the photocatalytic TiO2. | The optical properties measured using UV-visible spectrophotometer (Absorbance (A), energy band gap (Eg) and absorption coefficient ( α ) . TiO2 and TiO2- solid state reaction showed clear blue shift of the absorption band gap which were (2.8ev, 2.7ev, 2.25ev, 2.0ev) to )TiO2- NaBH4(550 ) ,TiO2-NaBH4 (750 ) , TiO2-AlLiH4 (500 ) and TiO2 -AlLiH4 (750 )) respectively. The structure of prepared TiO2 nanopowders were identified using XRD, particle size distribution varied appreciably in comparison with crystallite size (D) calculated from Sheerer formula which was in a good accordant compared with ASTM results , the particle size and their distribution were characterized using (AFM) . To the surface forms and compositions diameters of nanoparticles)SEM) was implemented . The energy dispersive X-ray (EDX) microanalysis was utilized to investigate the chemical composition of the whole samples. | Photocatalytic reaction was studied by using UV-Vis spectrophotometry. | In photocatalytic reaction the effect of the catalyst on photocatalytic rate of decomposition of methylene blue dye through the use of catalyst TiO2 and TiO2- solid state reaction (TiO2 - NaBH4 (550 ,750 )) and (TiO2 - AlLiH4 (500 ,750 )) . Using constant weight of the catalyst and dye. The most effective weight was found (1*10-4 M). At best weight the influence of many factors on rate of decomposition of dye were studied the impact of change pH varies (4.5, 7.1 and 9.4) found that the highest percentage in the decomposition of the MB was in the acidic media than in neutral and then alkaline. The effect of temperature variation from (20, 30, 40ºC) and found that increased rate of decomposition with increasing the temperature of the MB. Activation energy (Ea) for each reaction was calculated by using the equation of Arrhenius equation between (5.73-11.31) kJ mol-1 . | A series of dark reactions with absorbance measurement by UV-Vis spectrophotometry, within different periods of time with the change of pH and temperature. The results indicate that no degradation of the methylene blue dye although all the factors affecting in photocatalytic present except UV-light .
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: ماجستير
الموضوع الدقيق: الكيمياء
السنة: 2016
الموضوع العام: علوم الكيمياء
اسم المشرف: محسن عريبي الدخيلي ابراهيم عبود فليفل
اسم المؤلف: سراج علي رحيم

تحضير تشخيص والخصائص الكهربائية لبعض للليكاندات الجديدة المستندة على 4.3.1 اوكسادايزول، 4.3.1 ثايادايزول و 4.3.1 ترايازول ومعقداتها

المستخلص: The thesis include preparation and characterization of some new derivations of, 1,3,4-thiadiazole ,1,2,4-triazole and 1,3,4-oxadiazole as ligands that describe blowThe new complexes were prepared from the reactions of ligands L1, L2, L3, and L4 with transition metal salts (CrCl3.6H2O, FeCl3, CoCl2.6H2O and NiCl2.6H2O). | The elemental analysis (CHN), Infrared (IR) Spectroscopy, Nuclear magnetic resonance spectroscopy (1H NMR), Mass spectra magnetic Susceptibility and flame atomic absorption were used to characterize the structural formula of these ligands and their complexes. | Based on the results of the analytical and spectral measurements of the prepared complexes in this study, and compare them with literature in relation to coordinate sites in ligand. We can suggest the following shapes for the complexes : | 1- With regard to L1 we can conclude that its tridentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of three of the chloride ions, the geometric shape can be proposed to be octahedral geometry. For nickel (II) Complex the ligand acts as bidentate with two chlorine ions, the geometry is tetrahedral geometry (weak field ligand). | 2-for L2 we can conclude that its tridentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of three of the chloride ions, the geometric shape can be proposed to be octahedral geometry. For nickel (II) Complex, the ligand acts as bidentate with two chlorine ions, the geometry is square plainer geometry (strong field ligand). | 3 -for L3 we can conclude that it's bidentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of two of the chloride ions, the geometric shape can be proposed to be tetrahedral geometry. For nickel (II) Complex, the ligand acts as bidentate with two chlorine ions, the geometry is square plainer geometry (strong field ligand). | 4 - For L4 we can conclude that it is bidentate with [Cr (III), Fe (III) and Co (III)], In addition to the presence of two of the chloride ions with two molecule of ligand, the geometric shape can be proposed to be octahedral geometry. For nickel (II) Complex, the ligand acts as bidentate with two chlorine ions, the geometry is square plainer geometry (strong field ligand). | The study also examined the electrical conductivity for both of L1, L3 and their complexes with (Co(III), Fe(III), and Cr(III)) in the presence and absence of iodine. | The study showed that both L1 and L3 are semiconductors and the electrical conductivity of L1 is greater than that of L3. The complexes of these ligands has significantly increased their electrical conductivity and Iron complexes are the most complex electrical conductivity complexes. | As for iodine doping of ligands and their complexes, it was found that iodine increases the conductivity of ligands while decreasing the conductivity of the complexes. However, despite the decrease in the conductivity of the complexes, the conductivity is still higher than those of the free ligands. | A theoretical study for ligands (L1 and L3) and their complexes by Gaussian 09 program and calculate the total energy , HOMO ,LUMO and energy gap for all the studied compounds were found semiconductor
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: دكتوراه
الموضوع الدقيق: الكيمياء اللاعضوية
السنة: 2019
الموضوع العام: علوم الكيمياء
اسم المشرف: محسن عريبي الدخيلي ابراهيم عبود فليفل
اسم المؤلف: امل حسين نعيثل الزيدي

التحقيق في اثار الحجامة الرطبة على بعض المؤشرات البايوكيميائيه في ذي قار محافظة / العراق Investigation of The Effects of Wet Cupping Therapy on Some Biochemical Parameters in Thi - Qar Governorate/ Iraq

المستخلص: This study was designed to determine the effect of cupping to treat or reduce a lot of blood variables such as diabetes, liver failure, lipid profile and status of Oxidative and antioxidant , where we have in this study to take blood samples from the volunteers before they activate cupping therapy and then we have to take more samples within 14 days and comparing the results obtained were as follows : The results of the blood glucose concentration decreased significantly (P≤0.05) post cupping when compared with a pre-cupping, while there is no significant decrease in the level of glucose in the blood serum of a group post cupping compared with the control group (P≥0.05 ). In addition, the group pre-cupping showed a significant increase (P≤0.05) in the glucose in the blood serum when compared with the two sets of post-cupping and the control group. It can be seen the results of MDA serum showed a decrease (P≤0.05) in the group post cupping, compared with a pre-cupping, while non-significant in the serum level of MDA in the group post cupping compared with the control group (P≥0.05). While the group pre cupping significant (P≤0.05) MDA in serum when compared with the two sets of post-cupping and control. Summary | XIV | Cp serum levels showed high significant increase (P≤0.05) in | serum Cp can be observed in the two groups pre and post cupping when comparing this with the control group, In addition, the total post-cupping has shown a significant decrease (P≤0.05) in serum Cp compared with a pre-cupping. | As well as the results showed Alb serum significantly increased (P≤0.05) in Alb serum can be observed in the two groups pre and post cupping when compared with the control group, as a group post the cupping showed that there was a significant decrease | (P≤0.05) in Alb serum compared with a pre cupping. | Liver function tests showed a significant decrease in the group post cupping, compared with a pre cupping (P≤0.05), while significant difference was observed liver enzymes levels (ALT, ALP and AST) in the serum can be observed in a post-cupping compared with the control group (P≤0.05). Moreover, the group pre-cupping showed a significant increase (P≤0.05) in levels of ALT, ALP, AST serum when the two groups to be compared with the postcupping and the control group. | Fat results in the serum showed little change, but did not reach the moral (P≥0.05) in the proportion of fat in the blood serum levels of lipoproteins among all groups studied. | In the end we can say that cupping is not used for treatment once and for all, but it's used to treat Alternatively, or in a more identification used to treat complementary.
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: ماجستير
السنة: 2016
الموضوع العام: علوم الكيمياء
اسم المشرف: محمد عجة عودة
اسم المؤلف: زهراء طالب مشلول

طريقة كروماتوغرافية طيفية جديدة - لتقدير عقار اللوراتادين في بعض المستحضرات الصيدلانية Anew Chromatographic - Spectrophotometric Method for Determination of Loratadine in Some Pharmaceutical Preparations

المستخلص: Due to the medicinal significance of Loratadine, ethyl4-dihydro-11H benzo [5,6] cyclohepta [1,2-b] pyridin-11ylidene (-1-piperidinecarboxylate) has been devoted to this message To create a new chromatographic-spectral method for estimating the pure drug and the drug found in a number of its pharmaceuticals. | The letter included a detailed explanation of a new chromatographic-spectral method for estimating amounts of pure and commercial loratidine. The principle of this method is to break down the double bond present in the loratadine by the potassium permanganate oxidant factor of 0.05 molar and convert it into two ketone-containing compounds : 8-Chloro-5,6-dihydro-11H-benzo [5,6] cyclohepta [1,2-b The second compound is ethyl-4-oxopiperidine-1-carboxylate (B). It has been shown that the two compounds (A and B) can be separated by TLC, FTIR, separated and completely isolated by column chromatography technique. After the separation, the compound (A) was given a stable colorant complex with 4-amino acid benzoic acid ester, in a acidic medium, While the compound ( B ) did not give a stable complex. The results showed a study of changing the conditions of the process of analysis and separation of the two compounds and their diagnosis and the formation of the resulting complex and applications of the method and discussed with the use of different quantities of many types of acids and strong and weak rules and indicate their impact on the intensity of the complex complex color and the optimal conditions were selected for his way of work.
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: ماجستير
السنة: 2019
الموضوع العام: علوم الكيمياء
اسم المشرف: محمد تركي خثي
اسم المؤلف: صفاء حكيم ناصر الغزاوي

تخليق وتشخيص لبعض المركبات الحلقيه الغير متجانسه كالبيتا لاكتام والكاما لاكتام وفق تفاعل كانيكوزا SYNTHESIS AND CHARACTRIZAITION OF SOME NEW HETROCYCLIC COMPOUNDS INCLUDING ? & ? LACTAMS BY USING KINUGASA REACTION

المستخلص: This study is concerned with the synthesis and characterization of the some β- lactams 3(a-f),as in (Table.2). These compounds 3(a-f) were prepared by reacting phenylactylene with the appropriate nitrones2(a-f), in the presence of triethylamine | in acetronitrel under nitrogen atmosphere at -10˚C. in moderate yield (50-70)% . The nitrones compound 2(a-f) were prepared by reacting aldehyde with appropriate N-phenyl hydroxyl amine 1 in the presence of Ethanol. | As in (Table.1) Also the N-phenyl hydroxyl amine 1 compounds were prepared by reduction of nitrobenzene with ammonium chloride in Zinc Powder in the presence of water.This study is concerned with the synthesis and characterization of mono-γ- | lactams and bis-γ-lactams These compounds were prepared by reaction phenylsuccinic anhydride with the appropriate schiff bases(imines), by using chloroform solvent and heated at temperature (51-61˚C) in moderate yields(70- 92)%, All this compound confirmed by using spectra data such as : , IR , 1H-NMR , 13CNMR , APT 13C-NMR , HSQC 1H-13C-NMR,Mass
الصفحات الاولى:
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: ماجستير
الموضوع الدقيق: الكيمياء العضوية
السنة: 2016
الموضوع العام: علوم الكيمياء
اسم المشرف: محمود شاكر مكطوف محسن عريبي الدخيلي
اسم المؤلف: دعاء هادي محسن العطار

التاثير الوقائي للخلاصة المائية لاوراق نبات الزريج STZ على الكبد واعتلال الخصوبة في ذكور الجرذان المصابة بالسكري بواسطة Potential Role of Aqueous Extract From Chrozophora Tinctoria Leaves on Liver and Fertility Dysfunction in STZ Induced Diabetic Male Rats

المستخلص: This study was designed to investigate the pharmacological effects on air dried Chrozophora tinctoria (L.) Rafin plant samples as well as the responses of streptozotocin (STZ)-induced diabetic rats for the aqueous Chrozophora tinctoria (L.) Rafin leaves extracts. To achieve this aim, phytochemicals analysis were carried out by various standard assays and then antioxidant compounds contents in the three parts of the plant (leaves, stems, and roots) estimated by common spectroscopic methods. In addition, physiological, biochemical and histological parameters of (STZ) diabetic rats are evaluated too. Rats are distributed into five groups : Control, diabetic rats and three diabetic groups received orally different doses of (50, 70, and 90 mg/kg body weight (BW)) from the target extract for a period of 35 days. When the therapy is ended, blood samples, liver and testis tissues were taken and concentration of glucose, insulin, lipid profile, HbA1C, as well as the activity of ALT, AST, ALP, male sexual hormones were determined as well as liver and testis histology. In general, the results of this study show that the liver and testis tissue were damaged, serum ALP, AST ALT activities, HbA1C, lipid profile, T, LH, FSH, insulin and blood glucose levels were remarkable normalized. It was observed that the BW of diabetic control group is decreased. However the BW elevated slightly in the diabetic treated groups as well as serum insulin and male hormones. In addition, the extract improves the liver function and reduces lesions associated with diabetic state in STZ induced rats. Moreover, the effect of oral administration of Chrozophora tinctoria (L.) Rafin at a dose of 90 mg / kg body weight was more efficient than the 50 and 70 mg/kg body weight. Furthermore, the obtained results related that male reproductive system showed remarkable increased of sperm count, viability and motility after treatment with dose 70 mg/kg of body weight. Histological examination of the testis revealed improvement of spermatogenesis and Leydig cell proliferation with all doses of the extract. However, the histological features of the rats testis received 70 and 90 mg/kg, was found to be similar to the healthy group. The whole results indicated that the extract exhibited protective effect on liver tissues, as well as maintained the damage fertility in diabetic rats. These investigations explain its potentials as an antidiabetic, hepato protective agent, and promising therapeutic to recover male subfertility
الصفحات الاولى:
مكان الجامعة: ذي قار
اللغة: الانكليزية
الدرجة: دكتوراه
السنة: 2019
الموضوع العام: علوم الكيمياء
اسم المشرف: محمد عجة عودة
اسم المؤلف: منى حسون عبودي

تحضير وتشخيص مركبات حلقية غير متجانسة تحتوي على حلقات - 1,2,3ترايازول و - 1,3,4ثايادايزول Synthesis and Characterization of New Heterocyclic Compounds Containing 1,2,3 - Triazole and 1,3,4 - Thiadiazole Rings

المستخلص: تم في هذه الرسالة تحضير وتشخيص و دراسة الاستقراية الحرارية لسلسلة جديدة من مركبات حلقية غير متجانسة تحتوي على 3,2,1-ترايازول وحلقة 4,3,1-ثايادايزول ومجموعة الايمين (قواعد شف). تضمن الجزء الاول من البحث تحضير مشتقات 3,2,1-التراياازول 53-57 باستخدام تفاعل الاضافة الحلقية بين الازايد والالكاين بوجود مركبات النحاس الاحادي كعامل مساعد. لذا تم تحضير سلسلة من مركبات الازايد الاروماتي 48-52 كمكونة الازايد المطلوب في تفاعل الاضافة الحلقية بينما تم استخدام حامض البروباينويك المتوفر تجاريا كمكونة الالكاين. ان استخدام حامض البروباينويك في هذا التفاعل يؤدي الى تعويض حلقة 3،2،1-التراياازول بمجموعة كاربوكسيل وبالتالي يمكن استغلالها في الكثير من التفاعلات لتحضير مركبات مشتقات جديدة لتطبيقات مختلفة. | بعد تحضير مشتقات 3,2,1-الترايازول، تم التركيز على استغلال مجموعة الكاربوكسيل في تحضير حلقة4,3,1- ثايادايزول متجمعة مع حلقة 3,2,1-التراياازول وذلك من خلال مشتقات الترايازول 53-57 المحضرة مع ثايوسيمي كاربازايد بوجود زيادة من POCl3 وبالتالي الحصول على سلسلة جديدة من المركبات الحلقية الجديدة تحتوي على4,3,1- ثايادايزول متجمعة مع حلقة 3,2,1-الترايازول في جزيئة واحدة 53-57. بسبب احتواء المركبات الناتجة على مجموعة امين معوضه مباشرة على حلقة الثايادايزول في الموقع C2, لذا تم استغلال هذه المجموعة لتحضير سلسه جديده من مشتقات قواعد شف وذلك بالتفاعل مع اثنين من الالديهايدات الاروماتية بارا برومو بنزالديهايد وبارا نايترو بنزالديهايد. | وتم تشخيص جميع المركبات المحضرة بمقياس الاشعة تحت الحمراء FT-IR ومطيافية الرنين النووي المغناطيسي ومطيافية الكتلة. | علاوة على ذلك تم دراسة السلوك الحراري للمركبات المحضرة بتقنية التحليل الحراري الوزني | TGA والتحليل الحراري التفاضلي الوزني .DTG | == This thesis describes the synthesis, characterization and thermal study of new heterocyclic compounds containing 1,2,3-triazole, 1,3,4-thiadiazole and imine moieties at the same molecule. Firstly, the copper (I) catalyzed azide-alkyne cycloaddition (CuAAC) was the method choice for the synthesis of the target 1,2,3-traizole derivatives 53-57. Thus, a series of p-substitution phenyl azides 48-52 was designed as azido components of this reaction which was synthesized via reaction of diazonium salts with sodium azide. The propiolic acid was chosen as an alkyne building block in CuAAC reaction. Importantly, choosing propiolic acid as a second moiety of CuAAC reaction is allowed to functionalize the target 1,2,3-triazole derivatives 53-57 with a carboxyl group. The latter, can be exploited in different reactions and applications. The main efforts are focused to exploit their carboxyl function groups for the combination of 1,2,3-triazole ring system with 2-amino-1,3,4-thiadiazole ring system. However, new series of heterocyclic compounds containing 1,2,3-triazole and 1,3,4-thiadiazole moieties at the same molecule was synthesized through condensation reaction between the synthesized 1,2,3-triazole derivatives 53-57 with thiosemicarbazide in the presence of POCl3. Furthermore, as the synthesised compounds 57-62 containing an amino function group attached into the C2 position of 1,3,4-thiadiazole ring, it was exploited for the synthesis of new heterocyclic compounds containing 1,2,3-triazole, 1,3,4-thiadiazole and imine moieties in one molecule. All the synthesized compounds were characterized by the FT-IR, NMR and Mass spectroscopies. For further investigations, the thermal behavior of the synthesised compounds was studied by TGA and DTG techniques
الصفحات الاولى:
مكان الجامعة: المثنى
اللغة: الانكليزية
الدرجة: ماجستير
الموضوع الدقيق: الكيمياء
السنة: 2009
الموضوع العام: علوم الكيمياء
اسم المشرف: رياض جليل ناهي
اسم المؤلف: نور حميد عمران

تحضير وتشخيص مشتقات جديدة ل 1،2،3 ترايزول - المحتوية على 4،1،3 اوكسادايزول - ومجموعة الازو Synthesis and Characterization of New 1,2,3 - Triazole Derivatives Containing 1,3,4 - Oxadiazole and Azo Moieties

المستخلص: This thesis describes the synthesis, characterization and thermal study of new 1,2,3-triazole derivatives containing 1,3,4-oxadiazole and azo moieties. For the synthesis of the target 1,2,3-traizole derivatives 61-67, the copper (I) catalyzed azide-alkyne cycloaddition (CuAAC) was the method choice. Since the azide compounds being considered as a substrate for (CuAAC), a series of substituted phenyl azides was synthesized via reaction of diazonium salts with sodium azide, while the commercially available propiolic acid was chosen to be the alkyne function. Choosing of propiolic acid as an alkyne component of click reaction is allowed to functionalize the target 1,2,3-triazole derivatives with a carboxyl group function which can be exploited in different reactions and applications. Having the target 1,2,3-triazole derivatives 61-66, our efforts focused to exploit their carboxyl function groups for the synthesis of new heterocyclic compounds containing 1,3,4-oxadiazole moieties. A new series of compounds containing on 1,2,3-triazole and 1,3,4-oxadiazole moieties on the same molecule was synthesized through a condensation reaction between the synthesized 1,2,3-triazole derivatives 61-66 and semicarbazide hydrochloride followed by dehydro-cyclization step in the presence of POCl3. On the other hand, compound 67 was synthesized as an unnatural amino acid containing 1,2,3-triazole ring and is ready for different reactions such as diazonium salts formation. Thus, this unnatural amino acid was exploited in the synthesis of new three azo compounds following the standard procedure that is used in the synthesis of the azo compounds 74-73. The synthesized compounds introduce the 1,2,3-triazole and azo moieties on the same molecule thereby new applications can be reported. All synthesized compounds were characterized by the FT-IR, 1H-NMR, 13C-NMR and GC-MS spectroscopies. For further investigations, the thermal behavior of the synthesized compounds was studied by TGA and DTG techniques.
الصفحات الاولى:
مكان الجامعة: المثنى
اللغة: الانكليزية
الدرجة: ماجستير
الموضوع الدقيق: الكيمياء
السنة: 2019
الموضوع العام: علوم الكيمياء
اسم المشرف: رياض جليل ناهي
اسم المؤلف: زينب كزار كويت راضي

تحضير وتشخيص 4,1 - بس (اميدازول - 1 - يل مثيل) بنزين - سليكا ودراسة فعاليته كعامل مساعد Synthesis and characterization of 1,4 - bis (imidazole - 1 - yl methyl) benzene - silica and its catalytic activity

المستخلص: في هذه الدراسة تم استخلاص السيلكا من قشور الرز عن طريق غسل قشور الرز مرات عديدة بالماء المقطر، ثم عوملت مع محلول (1مولاري) من حامض النتريك، بعد ذلك احرقت في فرن بدرجة حرارة 800 درجة مئوية ، تم تحويل السليكا الناتجة الى سيليكات الصوديوم بعد ذلك تم مفاعلتها مع CPTES ينتج سليكا ذات مجموعة وظيفية --CH2Cl رمز لها بالرمز .RHACClتم تحميل الاميدازول المتفاعل مع كلوريد بارزاايلين على سطح .RHACClلتكوين العامل المساعد غير المتجانس رمز له .RHAPrIM تم تشخيص العامل المساعد بعدة تقنيات منها تحليل العناصر والتحليل الوزني الحراري TGA/DTA وتحليل امتزاز النتروجين ومطيافية الاشعة تحت الحمراء FT-IR وكذلك اطياف الرنين النووي المغناطيسي للحالة الصلبة لنواة ذرتي الكربون والسيليكون ( ( 29Si , 13C MAS NMRوكذلك المجهر الالكتروني الماسح SEM والمجهر الالكتروني النافذ.TEM طبقا الى نتائجCHN ،.EDXلوحظ زيادة نسبة الكربون اكثر مما هي عليه في RHACCl وبين التحليل كذلك وجود نسب من النتروجين والتي لم تكن موجودة سابقا في المركبRHACCl. اظهر تحليل الرنين النووي المغناطيسي للحالة الصلبة لنواة ذرة السيليكون29Si وجود ازاحات كيميائية تعود الى Q4،Q3 ، T3، T2 عند ازاحات كيميائية في الطيف حسب الادبيات. اما تحليل الرنين النووي المغناطيسي للحالة الصلبة لنواة ذرة الكربون13C اظهر حزما عند مواقع كيميائية مختلفة تعود لذرات الكربون في العامل المساعد المحضر. في حين بينت نتائج التحليل الحراري TGA/DTA امكانية استخدام العامل المساعد حتى 277 درجة مئوية دون ان يتفكك . وطبقا لصور المجهر الالكتروني النافذ TEM ظهرت دقائق ذات اشكال منتظمة وبحجم 5 نانومتر ، بعضها ملساء والاخرى كانت مسامية.درست الفعالية التحفيزية للعامل المساعدRHAPrIM في حمل ايون النتريت لتحضير حامض النتروز المستخدم في تحضير املاح الدايزونيوم . يعتبر حامض النتروز المادة الاساسبة لتحضير الاصباغ ، حيث حظرت اصباغ مختلفة عن طريق تفاعل الازدواج بين المركبات الاروماتية واملاح الدايزونيوم. شخصت الاصباغ المحضرة بواسطة تحليل العناصر، FT-IR واطياف UV-Vis . لوحظ تطابق النتائج العملية والمحسوبة لتحليل العناصر لمركبات الازو المحضرة. تم اعادة استخدام العامل المساعد عدة مرات و بثباتية عالية. == In this study, silica was extracted from rice husk via washing rice husk many time with distilled water, and then treated with 1.0 M of Nitric acid; finally, it was burned in an oven at 800 oC. The ash was converted to sodium silicate and reacted with chloropropyltriethoxysilane to form RHACCl. Imidazole with p-xylylene dichloride was loaded onto RHACCl in the form of p-xylylbisimidazole to form solid catalyst donated RHAPrIM. Various analytical techniques were well characterize the catalyst including CHN analysis, TGA/DTA, FT-IR, N2-adsorption desorption study, 29Si &13C MAS NMR spectra TEM, SEM and EDX. According to the CHN results, it was noticed that the carbon percentage increased from (11.70%) in RHACCl to (16.704%) in RHAPrIM; also the results were showed a present of nitrogen in RHAPrIM which was not present in RHACCl. Silicon solid-state nuclear magnetic resonance showed Q4, Q3, T3, and T2 chemical shifts at expected position. 13C spectrum showed different peaks at different chemical shifts related to the carbon structures of the organic moieties. Thermal analysis showed that the catalyst could be used safely up to 277 ºC. TEM images of RHAPrIM showed regularly shaped particles with an estimated size 5 nm. Some particle seems to be smooth in shape, while the others showed a porous shape. The catalytic activity of RHAPrIM was examined in-situ preparation of nitrous acid which was used in the preparation of diazonium salt. The RHAPrIM was used to produce nitrous acid via it’s reaction with nitrite ions. Nitrous acid is the key start materials for dyes preparation via diazonium salt. Coupling reaction of aromatic compounds was carried out with a diazonium salt to yield a mono azo dye. All dyes were characterized by elemental analysis, FT- IR, and UV-Visible spectra. Both calculated and found results of elemental analysis of prepared azo compound were match with each other. The catalyst was stable and regenerated within a simple experimental procedure
الصفحات الاولى:
مكان الجامعة: المثنى
اللغة: الانكليزية
الدرجة: ماجستير
الموضوع الدقيق: الكيمياء
السنة: 2009
الموضوع العام: علوم الكيمياء
اسم المشرف: قاسم محمد حلو
اسم المؤلف: نهلة غازي فهد

تحضير وتشخيص بعض مونيمرات وبوليمرت جديدة محتوية على حلقات غير متجانسة ودراسة خواصها الحرارية والفعالية البايولوجية Synthesis and Characterization of Some New Monomers and Polymers Containing Heterocyclic Rings and Study Their Thermal Properties and Biological Activity

المستخلص: يتضمن موضوع البحث تحضير مركبات حلقية غير متجانسة ثلاثية (الازردين و فنيل ازردين), خماسية (اوكسادايازول و ترايازول و تترازول), وخماسية ملتحمة (بنزوثايازول) والتي استخدمت لتحضير العديد من البوليمرات. | الجزء الاول : | يتضمن هذا الجزء تحضير مركب 2,3(1-ازردين)ماليك انهدريد[1] وبلمرته مع اثلين كلايكول و 1,3-بروبلين دايول و كليسيرول000الخ للحصول على رابطة استرية كما موضح بالشكل ادناه : | الجزء الثاني : | يتضمن هذا الجزء تحضير مركب 2,3(فنيل ازردين)ماليك انهدريد[12] وبلمرته مع اثلين كلايكول و 1,3-بروبلين دايول و كليسيرول000الخ للحصول على رابطة استرية كما موضح بالشكل ادناه : | الجزء الثالث : | يتضمن هذا الجزء تحضير مركب 3,2,ثنائي [2-مركبتو-5-يل-4,3,1-اوكسادايازول]1-ازردين [24] وبلمرته مع ثنائي كلوريدات الحامض للحصول على رابطة ثايواسترية كما موضح بالشكل ادناه : | الجزء الرابع : | يتضمن هذا الجزء تحضير مركب بنزوثنائي-2-امينوثايازول [29] وبلمرته مع ثنائي كلوريدات الحامض للحصول على رابطة امايدية كما موضح بالشكل ادناه : | الجزء الخامس : | يتضمن هذا الجزء تحضير مركب 4,1-ثنائي [3-مركبتو-4-(5-(بارا-فنيل)تترازولين)-5-يل-4,2,1-ترايازول] بيوتان [34] وبلمرته مع ثنائي كلوريدات الحامض للحصول على رابطة ثايواسترية كما موضح بالشكل ادناه : | * شخصت (المونمرات والبوليمرات) المحضرة باستخدام مطيافية FT.IR وUV/Vis و 1HNMR و 3CNMR وCHN كما قيست درجات انصهارها. | *درست اللزوجة و الصفات الحرارية لبعض البوليمرات المحضرة. | *كما تم تقييم الفعالية الحيوية لبعض البوليمرات المحضرة لتحديد امكانية استخدامها كمركبات ذات تطبيقات طبية. | == This work involves synthesis of different three (Aziridine, Phenyl azridine), five (Oxadiazole, Triazole, Tetrazole), and fused five (benzothiazole) member heterocyclic rings which used as a monomer for preparing many different polymers. | First part : | This part involves the synthesis of 2,3[1H-aziridine]maleic anhydride[1] and polymerized with ethylene glycol, 1,3-propylene diol, glycerol,…..etc. to get the polymers having ester linkage as shown below | This part includes the synthesis of 2,3[1-phenyl-aziridine]maleic anhydride[12] and polymerized with ethylene glycol, 1.3-propylene diol, glycerol,…..etc. to get the polymers having ester linkage as shown below This part includes the synthesis of 2,3-Bis[2-mercapto-5-yl-1,3,4-oxadiazole]1H-aziridine[24] and polymerized with diacid chlorides to get the polymers having thioester linkage as shown belowThis part contains the preparation of five member rings fused with benzene ring, its Benzobis-2-aminothiazole [29] and polymerized with diacid chlorides to get the polymers having amide linkage as shown belowIn this part, the compound 1,4- Bis[3-mercapto-4-(5-(p-substituted phenyl)tetrazolin)-5-yl-1,2,4-triazole]butane [37], [38] and polymerized with different diacid chlorides to get the polymers having thioester linkage as shown below In this part, the compound 1,4- Bis[3-mercapto-4-(5-(p-substituted phenyl)tetrazolin)-5-yl-1,2,4-triazole]butane [37], [38] and polymerized with different diacid chlorides to get the polymers having thioester linkage as shown below
الصفحات الاولى:
مكان الجامعة: بغداد
اللغة: الانكليزية
الجامعة: جامعة بغداد
الدرجة: دكتوراه
الموضوع الدقيق: الكيمياء
السنة: 2011
الموضوع العام: علوم الكيمياء
اسم المشرف: هلال مسعود عبد الله ابتسام خليفة جاسم
اسم المؤلف: غادة مهدي كامل الزبيدي

تخليق مشتقات سبيرو، حلقة ملتحمة و ايمين جديدة لسكر D - كلوكوفيورانوز على C - 3 ودراسة تاثيراتها على انزيمي | (ALP و GGT) Synthesis of New Spiro, Fused Ring and Imine Derivatives of D - Glucofuranose at C - 3 and Study Their Effect on Serum (ALP and GGT)

المستخلص: تم في هذه الدراسة تحضير مشتقات جديدة لسكر العنب وهذه المشتقات هي عبارة عن سبايرو، حلقة ملتحمة وٳيمين في الموقع رقم ۳. | ٳن معاملة السكر الحر الحاوي على مجاميع هيدروكسيلية مثل سكر الكلوكوز مع الاسيتون باستخدام حامض الفوسفوريك وكلوريد الخارصين كعوامل مساعدة يؤدي الى تكوين حلقتي اسيتال خماسية على الموقعين (١،٢)-(٥،٦) لسكر الكلوكوزليتكون المشتق(١،٢)-(٥،٦)-ثنائي-O-ايزوبروبلدين-α-D-كلوكوفيورانوز (٦٩). | ان لهذه المركبات المحمية اهمية كبيرة في مسارات تخليق مركبات متعددة كما في حالة الD- كلوكوز عند حماية مجاميع الهيدروكسيل على المواقع (١،٢)-(٥،٦) حيث تترك مجموعة الهيدروكسيل على الموقع ۳ حرة لتشترك التفاعلات. | اكسدة المشتق (٦٩) باستخدام ثنائي مثيل سلفوكسيد و انهدريد الخليك ليعطي المشتق (١،٢)-(٥،٦)-ثنائي-O-ايزوبروبلدين-α-D-هكسوفيورانوز-۳-يلوز (٣٨). | معاملة المشتق (٣٨) مع كاربوايثوكسي مثيلين ثلاثي فنيل فوسفورين في الاسيتونتريل يعطي المشتق ۳-دي اوكسي-۳-C-ايثوكسي كاربونيل مثيلين(١،٢)-(٥،٦)-ثنائي-O-ايزوبروبلدين-α-D-رايبوهكسوفيورانوز(٧٠). | معاملة المشتق(٧٠) مع هيدروكسيد الصوديوم والكلوروفورم بوجود بروميد الامونيوم رباعي البيوتيل كعامل مساعد ليعطي المشتق ٢،٢- ثنائي كلورو-٤-(١’،٢’- ثنائي هيدروكسي اثيل)- ٦،٧- ثنائي-O-ايزوبروبلدين-٥-اوكسا - سبايرو ٢]،٤ [ - هبتان-١-اثيل فورمات(٧١). | معاملة المشتق الكيتوني (٣٨) مع بارا ميثوكسي انيلين في الايثانول المطلق مع ٥ قطرات من حامض الخليك الثلجي يعطي المشتق۳- (٤- ميثوكسي فنيل ايمين)-(١،٢)-(٥،٦)-ثنائي-O-ايزوبروبلدين-α-D-كلوكوفيورانوز (٧٢). | حضر المشتق ١- (٢’،٢’- ثنائي مثيل- ١]،۳ [- داي اوكسالان-٤’- يل)- ۳،٤-ثنائي-O-ايزوبروبلدين-١١-(٤’-ميثوكسي فنيل)- ٢، ٦- ثنائي اوكسا-١١-ازا- سبايرو ٤]،٦ [-انديك-٨-ين-٧،١٠-دايون (٧۳) من تفاعل المشتق الاميني (٧٢) مع انهدريد الماليك باستخدام تفاعلات اضافةالحلقة. | حضر المشتق ]۳ ٨’(٤’’- ميثوكسي فنيل) ثنائي هيدرو-٦’-اوكسا-٨’-ازا-بنزوسايكلوهيبتين -٥’ ، ٩’- دايون [ - سبايرو ] ٤، ٦ [- (١،٢) - (٥،٦) - ثنائي - O-ايزوبروبلدين-α-D-كلوكوفيورانوز (٧٤) من تفاعل المشتق الاميني (٧٢) مع انهدريد الفثاليك باستخدام تفاعلات اضافةالحلقة. | تم الحصول على المشتق ۳،٦- انهيدرو-۳-(٤’- ميثوكسي فنيل امينو)-D- كلوكوفيورانوز (٧٥) بازالة الحماية من الموقعين ٥،٦ لاعطاء مشتق الحلقة الملتحمة. | تم دراسة تاثير المشتقات المحضرة (٧١ - ٧٥) على فعالية انزيمات الفوسفاتيز القاعدي (SALP) وانزيم نقل الكاما كلوتاميل (SGGT) في مصل الدم. | تم استخدام تراكيز مختلفة ( -٢ ١٠ - -٦ ١٠ مولاري) من المشتقات المحضرة وقد اظهرت نسب تثبيطية مختلفة على فعالية الانزيمين. النسبة المئوية للتثبيط تتناسب طرديا مع تركيز المشتقات. | تم احداث انواع مختلفة من التثبيط من قبل كل من هذه المشتقات على فعالية ALP و GGT . | اظهر المشتق (٧١) تاثيرا تثبيطيا لا تنافسيا للانزيمين واظهر المشتق (٧٤) تاثيرا تثبيطيا تنافسيا لانزيمي ال ALP و GGT ، بينما اظهرت المشتقات (٧٢)،(٧۳)،(٧٥) انواعا مختلفة من التثبيط لكل من الانزيمين ALP و GGT . | | == In this study, new derivatives of D-glucose have been synthesized. These derivatives are spiro, fused ring and imine at position-3. | Treatment of free sugar containing hydroxyl groups such as D-glucose with acetone using phosphoric acid and zinc chloride as catalyst led to the formation of two five memberd acetal ring; 1,2 : 5,6-di-O-isopropylidene-α-D-glucofuranose (69). | They were very useful in this synthetic routes as blocking groups and were used in the case of D-glucose for protecting the hydroxyl groups at C-1, C-2 and C-5 and C-6 leaving the hydroxyl group free at C-3 for further reactions. | Oxidation of (69) utilizing by using dimethyl sulphoxide (DMSO) and acetic anhydride mixture to give 1, 2 : 5, 6-di-O-isopropylidene-α-D-hexofuranose-3-ulose (38). | Treatment of derivative (38) with carboethoxymethylene triphenyl phosphorane [(Ph)3P=CHCO2Et] in acetonitrile gave 3 - deoxy - 3 - C - ethoxycarbonylmethylene - 1, 2 : 5, 6 - di - O -isopropylidene-α-D-ribohexofuranose (70). | Treatment of (70) with NaOH, CHCl3 and tetrabutyl ammonium bromide(TBABr) as a catalyst gave 1-ethyl formate-2, 2- dichloro-4- [ ( 1’, 2’-O-isopropylidene ) ethyl ] -6, 7-O-isopropylidene-5-oxa-spiro [2,4] heptane (71). | Treatment of the 3-keto derivative (38) with p-methoxy aniline in absolute ethanol and 5-drops of glacial acetic acid gave 3-( 4-Methoxy phenylimino )-1, 2 : 5, 6-di-O-isopropylidene-α-D-glucofuranose (72). | Derivative 1- [ ( 1’, 2’-O-isopropylidene ) ethyl ] -3, 4-O-isopropylidene -11- ( 4’- methoxy phenyl ) - 2, 6 - dioxa -11- aza -spiro [4,6] undec-8-ene-7, 10-dione (73) was synthesized from the reaction of imine derivative (72) with maleic anhydride using cycloaddition reaction. | Derivative 3[8’(4’’-Methoxy phenyl)-7, 8-dihydro-6’-oxa-8’-aza-benzocycloheptene - 5’, 9’-dione ] - spiro [4, 6] -1, 2 : 5, 6-di-O-isopropylidene-α-D-glucofuranose (74) was synthesized from the reaction of imine derivative (72) with phthalic anhydride using cycloaddition reaction. | Derivative 3, 6 Anhydro -3-(4’- methoxy phenylamino)-D-glucofuranose (75) was obtained by deprotection at positions 5 and 6 to give the fused ring derivative. | The effect of the synthesized derivatives (71), (72), (73), (74) and (75) were tested on the activity of serum alkaline phosphatase (SALP) and serum gamma glutamyl transferase (SGGT) to evaluate their biological activity. | Different concentrations (10-6-10-2 M) of the derivatives showed different percentage of inhibitions were directly proportional with the concentration of derivatives. | The derivative (71) showed noncompetitive inhibition on both enzymes, but derivative (74) showed competitive inhibition on both ALP and GGT, while the derivatives (72), (73) and (75) showed different types of inhibition on both ALP and GGT. |
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