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1、ReactionofElementalSiliconwithMethanolBull.KoreanChem.Soc.2009,Vol.30,No.3683SlurryPhaseReactionofElementalSiliconwithMethanolinthePresenceofCopper:DirectSynthesisofTrimethoxysilane††,‡‡†,*JoonSooHan,JooHyunCho,MyongEuyLee,andBokRyulYoo†OrganosiliconChemistryLaboratory
2、,KoreaInstituteofScienceandTechnology,P.O.Box131,Cheongryang,Seoul130-650,Korea.*E-mail:bryoo@kist.re.kr‡DepartmentofChemistry,GraduateSchool,YonseiUniversity,Seoul120-749,KoreaReceivedNovember25,2008,AcceptedJanuary19,2009Slurryphasereactionofelementalsiliconwithmetha
3、nolhasbeenstudiedinthepresenceofcopperusingasmallooamountofcuprouschlorideasanactivatorinDBT(dibenzyltoluene)atvarioustemperaturesfrom200Cto320C.Trimethoxysilane(1a)withaSi-Hunitwasobtainedasthemajorproductandtetramethoxysilane(1b)astheminorproduct.Thereactionworkedwel
4、lusinga0.5wt%CuClasanactivator.Theoptimumtemperatureforthisdirectosynthesisof1awas240C.Methoxysilaneswereobtainedin95%yieldwith81%selectivityto1afrom85%conversionofelementalsilicon.KeyWords:Copper,Silicon,Methanol,Trimethoxysilane,AlkoxysilaneIntroductionWehaveprevious
5、lyreportedthedirectsynthesisofhydro-silanesfromthedirectreactionofelementalsiliconwithaHydrosilaneswithSi-Hunithavebeenwidelyusedasmixtureofhydrogenchlorideandactivatedorganicchlorides1-41314startingmaterialsforsynthesizingorganosiliconcom-suchasi-propylchloride,dichlo
6、romethane,andchloro-15poundsthroughhydrosilylationwitholefininacademicandformtogiveSi-Hcontainingi-propyltrichlorosilane,bis-industrialfieldssinceitwasdiscoveredbyJ.L.Speierin(chlorosilyl)methanes,andtris(chlorosilyl)methanes,respec-2161957thatahexachloroplatinicacidin
7、i-propylalcoholwasatively.ThissuccessinthedirectsynthesisofnewSi-H3,4veryeffectivecatalystforhydrosilylation.Eventhoughcontainingorganochlorosilanespromptedustoapplytothe5hydrochlorosilaneshasalongsynthetichistoryandbeendirectreactionofelementalsiliconwithmethanolgivin
8、g1well-establishedinacademicandindustrialfiled,theyreactsmethoxysilanes,trimethoxysilanewithaSi-Hunit(1a)andeasilywit
