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1、SupportingInformation©CopyrightWiley-VCHVerlagGmbH&Co.KGaA,69451Weinheim,2012SupportinginformationTheReactionofTertiaryAnilineswithMaleimidesunderVisibleLightRedoxCatalysisXuhuiJu,DianjunLi,WeifeiLi,WeiYu*andFenglingBian*StateKeyLaboratoryofAppliedOrganicCh
2、emistry,LanzhouUniversityLanzhou,P.R.ChinaFax:+86-931-8912582;Email:yuwei@lzu.edu.cn;bianfl@lzu.edu.cn113TheHandCNMRspectrawererecordedonaBrukerAM-400MHzspectrometer.TheEI-MSspectraweremeasuredonanHP5988Aspectrometerbydirectinletat70eV.Thehighresolutionmass
3、spectra(HRMS)weremeasuredonaBrukerDaltonicsAPEXII47espectrometerbyESI.MeltingpointsweremeasuredonanXT-4meltingpointapparatusandwereuncorrected.Flashcolumnchromatographywascarriedoutwithsilicagel(300-350mesh).FluorescencequenchingwasrecordedusingaPerkin1Elme
4、rLS55Luminescencespectrometer.N,N-Di(trideuteriomethyl)anilineand2N-methyl-N-trideuteriomethylanilinewerepreparedaccordingtoliteratures.GeneralprocedureforthereactionsoftertiaryanilineswithmaleimidesToa10mLroundbottomflaskequippedwithadryingtube(filledwitha
5、nhydrousCaCl2)andmagneticstirringbarwasaddedtertiaryaniline(1)(0.5mmol,2.0equiv.),maleimide(2)(0.25mmol,1.0equiv.),photocatalyst(0.0088mmol,0.035equiv.)andDMF(3mL).Thesolutionwasirradiatedunderstirringwithtwo40Whouseholdfluorescentlamps(distanceapp.4cm)atro
6、omtemperature.Afterthereactionwascomplete(indicatedbyTLC),thereactionmixturewasdilutedwithEtOAc(10mL),andpouredintosaturatedaqueousNH4Clsolution(15mL).TheaqueouslayerwasextractedwithEtOAc(10mL×3).Thecombinedorganiclayerswerewashedwithbrine(15mL×4)anddriedwi
7、thanhydrousNa2SO4.Thesolventwasremovedunderreducedpressure,andtheresidualwastreatedwithsilicagelchromatographytogivepureproduct(s).Compounds3couldbefurtherpurifiedbyrecrystalizationfrom1DCMandhexane.EmissionQuenchingExperiments.AllRu(bpy)3Cl2solutionswereex
8、citedat452nmandtheemissionintensityat609nmwasobserved.Inatypicalexperiment,anappropriateamountof0.025MsolutionofRu(bpy)3Cl2inDMFwasaddedtoasolutionofappropriateamountofquencherinaquartzcuvette(Theconce
