氯甲基水杨醛合成.doc

氯甲基水杨醛合成.doc

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时间:2021-02-11

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1、SupportingInformationforTetheringofCu(II),Co(II)andFe(III)tetrahydro-salenandsalencomplexesontoamino-functionalizedSBA-15:EffectsofsalenligandhydrogenationoncatalyticperformancesforaerobicepoxidationofstyreneYingYanga,YingZhangb,ShijieHaob,QiubinKanaaCollegeo

2、fChemistry,JilinUniversity,Changchun130023,Jilin,PRChinabDepartmentofMaterialsScienceandEngineering,ChinaUniversityofPetroleum,ChangpingDistrict,Beijing,102249,PRChinaSyntheticprocedures:1.PreparationofpuresiliceousSBA-15Typically,2.0gtriblockcopolymer(P123)w

3、asdissolvedin60mlof2.0mol/lHCland15mlofdistilledwaterat40oC,andthenthemixturewasstirredfor1h.Afterthat,4.17mloftetraethoxysilane(TEOS)wasadded.ThegelcompositionP123:HCl:H2O:TEOSwas0.017:5.88:197:1inmolarratio.Theresultingmixturewasfurtherstirredat40oCfor5h,an

4、dthentransferredintoateflon-linedstainlesssteelautoclaveandagedat100oCfor24h.Aftercoolingdowntoroomtemperature,theproductswerefiltered,washedwithdistilledwaterrepeatedly,anddriedovernightat60oCinair.Theas-synthesizedsamplewascalcinedat550oC(heatingrate1oC/min

5、)for16htoremovethecopolymertemplate.2.Preparationofamino-functionalizedSBA-151.0gofcalcinedSBA-15(pre-driedat120oCfor2h)wasaddedto100mlofdrytolueneina250mlflask,andtheflaskwasflushedwithnitrogenfor20min.Then0.54mlof3-aminopropyltriethoxysilane(APTES)wasaddeda

6、ndstirredfor24h.Thenthesolidwasfiltrated,washedwithtolueneandethanol,anddriedinair.AndthereceivedsolidwasdenotedasAPS-SBA-15.FoundforAPS-SBA-15:C,5.37;H,1.41;N,1.39%.FTIR(KBrpellets,cm-1):1510(NH2),1130-1000(Si-O-Si),960(Si-OH),687(N-H).3.Synthesisof5-chlorom

7、ethylsalicylaldehyde(5-CM-Sal)5-chloromethylsalicylaldehydewassynthesizedfromsalicylaldehydebytheclassicalchloromethylationmethod.Inatypicalsynthesis,17.5g(160mmol)ofsalicylaldehydewastreatedwith24mlof38%aqueousformaldehydeand1.2gofZnCl2in100mlofcon.HCl.Themi

8、xturewasstirredatroomtemperatureunderN2atmospherefor24h.Theresultingwhitesolidwasfilteredandrepeatedlyextractedwithdiethylether.ThecombinedorganicphaseswerewashedwithsaturatedaqueousNaHCO

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