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1、SupplementaryMaterialforChemicalCommunicationsThisjournalis©TheRoyalSocietyofChemistry2004Microwave-AssistedNegishiandKumadaCross-CouplingReactionsofArylChlorides·ElectronicalsupplementaryinformationGeneralconditions:·Tetrahydrofuran(THF)wasdriedbydistillingfromsodium-benzophe
2、noneketylunderargonatmospherepriortouse.N-methyl-2-pyrrolidinone(NMP,anhydrous99.5%,Aldrich,Cat.No.:32,863-4)usedasreceived.·Allstartingmaterialswerepurchasedfromcommercialsourcesandusedasreceivedorweresynthesizedasdescribedinthecitedreferences.·Magnesiumturningsfromoldersourc
3、ewerewashedwithdilutedaqueousmuriaticacidtillsilverlikeappearanceoccurred(around10minutes),filtered,washedwithethanolandfinallywithether.Driedat20mbarat50°Cforcirca30minutes.·TLCanalysiswasperformedonMerckprecoated60F254plates.·Flashcolumnchromatographywasperformedusingsilicag
4、el60(0.040-0.063mm,Merck).VisualizationperformedbyUVlightat254nm.·MeltingpointswereobtainedonaGallenkampmeltingpointapparatus,modelMFB-595inopencapillarytubesandwereuncorrected.·1H-NMRspectrawererecordedonaBrukerAMX360instrumentinCDCl3orDMSO-d6,operatingat360MHz.Chemicalshifts
5、arereportedinδvalueswithrespecttoresidualproton(1H)inthesolvent.·MassspectrawereobtainedonaHewlett-PackardLC/MSD1100seriesinstrumentintheatmosphericpressurechemicalionization(negativeorpositiveAPCI)mode.·GC/MSmeasuredonaHP6890apparatusequippedwithHP5mscolumn(30m,250μmi.d.,1μmf
6、ilmthickness)andaHP5973massselectivedetector.·HPLC-UVanalyseswereperformedinShimadzuSCL-10AapparatusconsistingofLC10-AT(VP)pumps,anautoinjector(S-10AXL),andadualwavelengthUVdetector(SPD-10A)setat215and280nm.Column”30-100-10LiChrospherâ100x3mm,RP-18(particlesize5μm),Merck,Cat.N
7、o.:51232”.Separationconductedbygradientelution,Acetonitrileandwaterwereusedaseluents.·CentrifugeVARIFUGE3.0,Heraeus-Sepatechused.·UltrasoundcleaningbathBandelinSonorexRK31used.·AllmicrowaveirradiationexperimentswerecarriedoutusingtheEmrysÔSynthesizerfromPersonalChemistryAB(Upp
8、sala).Allexperimentswerecarriedoutinsealedmicrowaveprocessvia
