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Microwave Irradiation for Organic Synthesis and Preparation of Albothyl

Author: HouMin
Tutor: LiZhiLiang
School: Chongqing University
Course: Analytical Chemistry
Keywords: Microwave radiation Perkin reaction Knoevenagel Reaction Experimental Design Policresulen
CLC: O644.2
Type: Master's thesis
Year: 2002
Downloads: 175
Quote: 1
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Abstract


Microwave chemistry is the use of modern microwave technology to study the physical and chemical behavior of substances in the microwave field under a new cutting-edge interdisciplinary microwave Organic Chemistry is an important branch in the field of microwave chemistry. In just ten years time, the microwave organic chemistry has been developed by leaps and bounds, so far studied and achieved obvious effect of microwave organic synthesis reactions involving almost each of the major areas of organic synthesis reaction. The microwave synthesis technology including microwave closed synthesis reaction technology, microwave atmospheric synthesis reaction under microwave synthesis reaction and microwave continuous synthesis reaction technology. Of microwave and pressure synthesis reaction technology, combined with orthogonal, uniform, trial design and intuitive analysis, analysis of variance, multiple linear regression, stepwise regression method, Perkin (Perkin) reaction and Knoevenagel (Cinu, text Nagel) The reaction was more in-depth studies to prove that the technology compared to traditional heating methods, fast heating, temperature uniformity of heating system, synthetic high yield and easy purification characteristics. The same time, the author of four new drugs policresulen \. The main content of this paper and the results are as follows: (1) examines the Perkin reaction to traditional heating method and microwave irradiation synthesis of cinnamic acid catalyst, microwave power and reaction time on the yield of cinnamic acid. Microwave Irradiation Synthesis of cinnamic acid in a yield of 40.44%, yield close to the conventional heating method (40-50%), but the reaction time of only 10 minutes was significantly reduced compared to the conventional heating method (1.5h). Which reflects the characteristics of microwave radiation can accelerate organic reactions. (2) orthogonal, uniform, experimental design to study the impact of the Knoevenagel reaction the molar ratio of raw materials and reagents, catalysts, microwave power and reaction time and other factors on the yield of cinnamic acid. Through the use of visual analysis, analysis of variance, multiple linear regression analysis and stepwise regression analysis of the experimental data processing, the best experimental conditions. Under this condition, the yield of the cinnamic acid reached 67.17%, yield (40-50%) higher than that of conventional heating method. In addition, the use of microwave radiation technology synthesized a series of beta-substituted acrylic acid, its production rate is close to or higher than conventional heating method. The results showed that microwave technology for the synthesis of acrylic acid beta-replace, easy to operate, quick response, high yield, easy purification product, has a certain value. (3) The synthesis method reported four new drugs for Patent the \dihydroxy -5,5 '- methylene bis (4 - methylbenzenesulfonate) piperazine, 2,2' - dihydroxy -5,5 '- methylene-bis (4 - methylbenzenesulfonate) sodium and other intermediate products, final compositing target product of 2,2 '- dihydroxy-5,5' - methylene-bis (4 - methyl-benzenesulfonate). Purity and structure of homemade refined products through the use of high performance liquid chromatography, infrared spectroscopy, ultraviolet spectroscopy, nuclear magnetic resonance spectroscopy analysis, confirmatory product is pure policresulen.

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CLC: > Mathematical sciences and chemical > Chemistry > Physical Chemistry ( theoretical chemistry ),chemical physics > Photochemical,radiation chemical,ultrasonic,the role of chemical processes > Radiation Chemistry
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