Microwave Irradiation For Organic Synthesis And Preparation Of Albothyl

Microwave Chemistry is a new subject, which investigates physical and chemical behavior of various matters. Microwave-Induced Organic Synthesis is an important branch of Microwave Chemistry. At the present time, microwave synthesis technique includes microwave sealed synthesis technique, microwave ordinary pressure synthesis technique, microwave dry medium synthesis technique and microwave continuous synthesis technique. In this thesis, microwave ordinary pressure synthesis technique has been employed in organic reactions. Experimental designs together with regression methods were used to investigate Perkin reaction and Knoevenagel reaction. It proved that the reaction systems under microwave irradiation reacted faster and gave higher yield than those under ordinary heating method. At the same time, the synthesis method and route of Albothyl (also Policresulen) has been investigated. The product was purified and its structure has been analyzed and proved to be true. The main contents and some conclusions are shown as follows:1.Perkin reaction under traditional heating method and microwave irradiation method was investigated. Influence of catalysts, microwave power and reaction time on the yield of cinnamic acid was investigated. The yield of cinnamic acid under microwave irradiation method was 40.44% and close to that in traditional heating method (40-50%). But the reaction time is only 10 min while it was 1.5 hours under traditional heating method. It proved that microwave irradiation technique could accelerate organic reactions.2.Orthogonal experimental design, uniform experimental design and central composition experimental design were used to investigate Knoevenagel reaction. The influence of molar ratio of benzaldehyde and malonic acid, power of microwave, reaction time and dosage of the catalysts on the yield of cinnamic acid was investigated mainly. Multiple linear regression method, and step regression method were used to process the experiment data. The optimum reaction condition was achieved. Under the optimum condition the yield of cinnamic acid was 67.17%, which was higher than the yield (40-50%) obtained under traditional heating method. And besides, a series ofβ-substituted crylic acids were synthesized in a similar way. And the yields were closed to traditional yields. In summary, microwave irradiation technique promoted Knoeveangel reaction with high yield and convenient operation. 3.The preparation methods of Albothyl has been investigated and improved. High performance liquid chromatography was employed to analyze the purity of the product. And infrared, ultraviolet, nuclear magnetic resonance was employed to analyze the refined product. And it was proved to be pure.