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Investigation On Intramolecular Cyclization Catalyzed By MCM-41Microreactors With The Different Pore Size

Posted on:2013-02-10Degree:MasterType:Thesis
Country:ChinaCandidate:J ZhuFull Text:PDF
GTID:2234330392453953Subject:Medicinal chemistry
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In recent years, the synthesis and application of various Organic-inorganicchemical mesoporous molecular sieve MCM-41have been studied deeply. We oftenuse MCM-41molecular sieves as the carrier of numerous catalysts to implement theorganic reaction because they have a variety of properties such as uniform Pore size,large specific surface area (>1000m~2/g) and larger adsorption capacity (>0.7cm~3/g),and the Surface silicon hydroxyl groups are easily be changed by functional group andso on. The traditional methods of changing the MCM-41microreactor pore size areextensive which include adjusting carbon chain length of the surface-active agent andthe optimization of post-processing process,etc. However, all these methods have thedrawbacks of long reaction time, harsh reaction conditions, complicated Post-processing.1,3,5-three methyl benzene (TMB) has been used as swelling agent in this dissertation,Four different pore size of MCM-41were prepared successfully by changing thenumber of swelling agents under the condition of microwave radiation.Comparig to conventional methods, microwave-assisted synthesis have a numerousadvantages such as accelerate reaction speed, improve the production rate, reduce theby-products and it can also promote the reactions which can not occur in conventionalconditions. We have investigated the yield of the synthesis of benzofuran-2(3H)-one andacridin-9(10H)-one using Four different pore size MCM-41microreactor as catalystsunder microwave radiation and conventional heating conditions. There are three parts inthis dissertion.In the first part, the synthesis of benzofuran-2(3H)-one and acridin-9(10H)-onewere studied under the microwave radiation and conventional heating in seven differentsolvents, which were described in the section two and section three. we have obtainedthe optimum condition of preparing benzofuran-2(3H)-one and acridin-9(10H)-onethrough comparing the effects of different solvents, different temperature and differenttime in yields.In the second part, we successfully obtained four different pore size mesoporousmaterials of MCM-41with the pore diameters3.7nm,4.6nm,5.4nm,7.2nmrespectively by changing the proportion of1,3,5-three methyl benzene (TMB) undermicrowave radiation. It was found that the four MCM-41have the structures andproperties of MCM-41such as characteristic absorption peak,uniform pore size, inerratic channel and the six-party ordered arrangement of the channel.In the third part, we used four different pore size MCM-41microreactors ascatalysts to promote the reaction yield of benzofuran-2(3H)-one and acridin-9(10H)-one.The objects are characterized by IR,1HNMR and mass spectrum. The yields inmicrowave radiation and conventional heating conditions show that the smaller the poresize was, the more excellent of catalysis were.
Keywords/Search Tags:MCM-41, microreactor, microwave benzofuran-2(3H)-one, cridin-9(10H)-one
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