Document Details
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Document Type |
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Thesis |
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Document Title |
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Chitosan Decorated Nanoparticles for One-Pot Synthesis of Fine Chemicals الكيتوزان المزين بالجسيمات النانوية للتحضير الأحادي للكيماويات الدقيقة |
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Subject |
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Faculty of Science |
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Document Language |
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Arabic |
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Abstract |
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In conclusion, in this study we have used the chitosan as a polysaccharide supported copper nanoparticles (NPs) catalyst to achieve our goals which represented in the synthesis of quinoline derivatives, which was carried out in several steps:
• A literature survey was carried out for the study of copper nanoparticles and chitosan in terms of properties, methods of preparation, characterization and applications.
• A literature survey was carried out for the study of quinoline and quinoline derivatives synthesis including classic methods and advanced methods.
• chitosan decorated copper NPs catalyst was synthesized through two reduction methods, a green protocol method and ionotropic gelation one. Two different precursors of Cu ions, copper (II) nitrate and copper (II) acetate, were used.
• Quinoline derivatives was mythized via (MCR) consist of four-component one-pot reaction of dimedone, pchlorobenzaldehyde, ethyl cyanoacetate and ammonium acetate. Neat reaction (absence of catalyst) showed ~25% yield in 6 h using ethanol under refluxing condition. The neat reaction carried out under ultrasonic irradiation resulted in poor isolated yield of the product (~29%) in 15 min.
• Based on previous results, the ultrasonic irradiation method was selected according to the advantages of this method in comparison to the conventional one in enhancing the product yield in shorter reaction time.
• In order to find out suitable chitosan decorated copper NPs catalyst, for the synthesis of quinoline derivatives via MCR under ultrasound irradiation, four different catalysts ,
CS/CuNPs A , CS/CuNPs N, CS/CuNPs/TPP A and CS/CuNPs/TPP N, were synthesized and tested. The effect of mass of the four catalysts was studied and the results clearly showed that 0.1 g of Cu-Cs NPs provided high product’s yield (~90 %) relative to the other catalyst under the same reaction conditions.
• A variety of quinolones derivatives were also synthesized via MCR under ultrasound irradiation by using the highly efficient catalyst (CS/CuNPs A).
• The catalyst provides an efficient synthesis of a new quinoline derivatives with high yield productivity, in short reaction time. In addition, the TON and TOF values were calculated and a remarkably high TON and TOF values were found with small mass of catalyst.
• Catalyst characterization was carried out by using FTIR, XRD, TGA, HRTEM, SEM-EDS, and XPS techniques.
• The Characterization of Catalyst showed the following:
• FT-IR spectra displayed new intense peaks in the fingerprint region at low –frequency (600-500 cm-1) due to formation of Cu−N and Cu−O coordinate bonds .
• XRD results showed CS patterns only without single pattern for copper NPs.
• The TGA thermogram of investigated samples display three mass loss stages.
• SEM image displayed asymmetrical deposits of chitosan flakes.
• XPS showed confirmed the presence of copper, which is not appeared in XRD patterns.
• TEM images showed Cu NPs are well dispersed over chitosan which were in two faces (111) and (110) .
• The catalyst was recycled for many times without substantial change in catalytic performance.
• Finally, the catalyst is a promising for the synthesis of novel quinoline derivatives of expected biological activity. The obtained results could open the gate towards promising noble metal free catalyst for fine chemical products utilizing green protocol. |
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Supervisor |
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Prof. Dr. Mohamed Mokhtar Mohamed Mostafa |
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Thesis Type |
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Master Thesis |
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Publishing Year |
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1440 AH
2019 AD |
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Co-Supervisor |
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Dr. Dina Abed Bakhotmah |
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Added Date |
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Sunday, May 5, 2019 |
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Researchers
| خديجة سعد الغامدي | Al-Ghamdi, Khadijah Saad | Researcher | Master | |
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