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Investigation On Synthesis Of 1- Indanone By MCM-41 Microreactor And Zeolite Microreactor

Posted on:2016-12-17Degree:MasterType:Thesis
Country:ChinaCandidate:Q LiuFull Text:PDF
GTID:2271330479485240Subject:Medicinal chemistry
Abstract/Summary:PDF Full Text Request
Micro-reactor is an important branch of supramolecular chemistry, it draws comprehensive attention since 1987 it has been raised. In recent years, micro-reactor has being used in the synthesis methodology because of highly catalytic activity and selectivity. The micro-reactor include:cyclic ligands hole, molecular aggregates and potous solid. Mesoporous is among one of porous solid reactors, which has been widely used in the fields of catalysis, sieving, adsorption, etc, owing to the advantages of high internal surface area, high pore volume and favorable, controllable pore uniformity and easy-doped structures. Meanwhile, it features simply after-processing and recycling favorability to the environment characters comparing to the traditional catalysts. Based on these features, this article demonstrates a method which uses mesoporous material as a micro-reactor to synthesis of 1-indanone.The first part of the article will explore Synthesis of 1-indanone in zeolite (Scheme 1). The traditional synthetic routes show that zeolite or modified zeolite used as catalysts and synthesis of 1-indanone in solution. The obvious drawbacks are that it requires long hours and very strict reactive condition and results in complicated post-process ing and low output rate, 1-phenyl-2-propen-1-ones is widely used because its high activity. This work adopts the 3-phenyl as raw materials, zeolite as reactor. The reaction conditions including temperature, reaction time, reaction vessel, eluent, the optimized conditions were obtained. When petroleum ether as solvent, the reaction temperature was 200 ℃, the reaction time is 6h and methanol as the eluent, yield 71.3%. Compared with the traditional method, zeolite as a micro-reactor can increase the yield of the product, decrease the reaction time. Proton acid center be the center of zeolile,acylation reaction mechanism of zeolite is dearelectrical substitution mechanism.The second part of the article mainly discusses synthesis of 1-indanone in MCM-41 with 3.7nm aperture. first of all, There are two methods to characterize the structures of MCM-41, such as XRD diffraction and nitrogen adsorption desorption. It was found that the MCM-41 has the structures and properties of MCM-41 such as characteristic absorption peak,uniform pore size, inerratic channel and the six-party ordered arrangement of the channel. Secondly The reaction conditions including temperature, reaction time, microwave radiation were investigated and the optimized conditions were obtained. Similarly with petroleum ether as solvent, methanol as eluent, the reaction temperature is 22℃, the reaction time was 8h, yield 63.4 Compared with zeolite, the yield of 1-indanone decreased slightly but still higher than traditional catalytic method.
Keywords/Search Tags:micro-reactor, MCM-41, Molecular sieves type 13X, 3-phenyl propionate, 1-indanone
PDF Full Text Request
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