photophysics,aggregationandamplifiedquenchingofa

photophysics,aggregationandamplifiedquenchingofa

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时间:2018-07-12

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1、SupplementaryMaterial(ESI)forChemicalCommunicationsThisjournalis©TheRoyalSocietyofChemistry2002Photophysics,AggregationandAmplifiedQuenchingofaWater-Solublepoly(PhenyleneEthynylene)C.Tan,M.R.PintoandK.S.Schanze,SupportingInformationThesyntheticapproachesusedtoobtai

2、nPPE-SO3-andPE-SO3-areoutlinedinSchemes1and2respectively.Scheme1Scheme23SupplementaryMaterial(ESI)forChemicalCommunicationsThisjournalis©TheRoyalSocietyofChemistry2002StartingMaterials2,5-Diiodohydroquinoneand1,4-diethynylbenzeneweresynthesizedaccordingtoprocedures

3、publishedelsewhere.1,2Monomer17.24g(20.0mmol)of2,5-diiodohydroquinonewasdissolvedinasolutionthatcontained2.0g(50.0mmol)ofsodiumhydroxydein200mLofwaterinaErlenmeyerflaskunderargon.Asolutionof6.1g(50.0mmol)of1,3-propanesultonein40mLofdioxanewasaddedtotheformersolutio

4、natonce.Theresultingmixturewasthenstirredatroomtemperatureovernight,duringwhichtimeathickpinkslurryformed.Thereactionmixturewasthenstirredat80-100°Cforanother30minutesandthencooledinawater/icebath.Thesuspensionobtainedwasvacuumfiltered,andtheretainedsolidwaswashedw

5、ithcoldwaterfollowedbyacetone,andcrystallizedtwicefromwater.Yield9.2g(70%)asafinewhitepowderC12H14I2Na2O8S2(Mol.Wt.:650.16):Analysiscalc:C22.17;H2.17;I39.04;S9.86Analysisfound:C22.43;H2.57;I34.63;S8.96FTIR(nmax.cm-1,KBrpellet):2975,2940,2872,1624,1489,1464,1438,139

6、0,1353,1262,1206,1156,1061,1032,937,850,795,739,629,5511H-NMR(DMSO-d6;dppmfromTMS):2.00(t,4H);2.64(t,4H);4.05(t,4H);7.30(s,2H)13C-NMR(DMSO-d6;dppmfromTMS):25.37,48.14,68.96,86.99,122.44,152.30PPE-SO3-1.008g(1.55mmol)ofmonomer1and0.189g(1.50mmol)of1,4-diethynylbenze

7、neweredissolvedinamixtureof20mLofwaterand20mLofDMFat60°CinaSchlenkflaskwithagentleflowofargonandwithmagneticstirring.Theresultingclearsolutionwasdeoxygenatedbyseveralcyclesofvacuum-argoncycling.Anothersolutioncomprisedof52.0mg(45.0μmol)ofPd(PPh3)4and10.0mg(45μmol)o

8、fCuIinamixtureof10mLofdiisopropylamineand10mLofDMFwaslikewisedeoxygenatedandwassubsequentlyaddedtotheformersolutionbymeansofacannula.Thefinalmixt

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