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1、SupportingInformationFor:Iron-CatalyzedCross-CouplingofPrimaryandSecondaryAlkylHalideswithArylGrignardReagents,†,‡††,†MasaharuNakamura,*KeikoMatsuo,ShingoIto,andEiichiNakamura*†DepartmentofChemistry,TheUniversityofTokyo,Hongo,Bunkyo-ku,Tokyo113-0033,Japan‡PRESTO,JapanSc
2、ienceandTechnologyAgency(JST)General.Allthereactionsdealingwithairormoisturesensitivecompoundswerecarriedoutinadryreactionvesselunderapositivepressureofargonornitrogen.Air-andmoisture-sensitiveliquidsandsolutionsweretransferredviasyringeorstainlesssteelcannula.Analytica
3、lthin-layerchromatographywasperformedusingglassplatespre-coatedwith0.25-mm230–400meshsilicagelimpregnatedwithafluorescentindicator(254nm).Thinlayerchromatographyplateswerevisualizedbyexposuretoultravioletlight(UV)and/orbyimmersioninanacidicstainingsolutionofp-anisaldehy
4、defollowedbyheatingonahotplate.Organicsolutionswereconcentratedbyrotaryevaporationat~15Torr(evacuatedwithadiaphragmpump).FlashcolumnchromatographywasperformedasdescribedbyStilletal.,1employingKantoSilicagel60(spherical,neutral,140-325mesh).Materials.Commercialreagentswe
5、repurchasedfromTokyoKaseiCo.,AldrichInc.,andothercommercialsuppliersandwereusedeitherdistilledorrecrystallizedbeforeuse.Anhydroustetrahydrofuran(THF)waspurchasedfromKantoChemicalCo.anddistilledfrombenzophenoneketylat760Torrunderanargonatmosphereimmediatelybeforeuse.Thew
6、atercontentofthesolventwasconfirmedwithaKarl-Fischermoisturetitratortobelessthan20ppm.FeCl3purchasedfromKantoChemicalCo.,wasdehydratedbySOCl2,anddriedthoroughlyunderreducedpressure,andtheresultingunhydrousFeCl3wasstoredunderargon.A0.1-MTHFsolutionofFeCl3tendstoformpolye
7、thercompoundsuponroom-temperaturestoragefordays,andthus,waspreparedimmediatelybeforeuse.(1)Still,W.C.;KIahn,M.;Mitra,A.J.Org.Chem.1978,43,2923–2924.S11Instrumentation.Protonnuclearmagneticresonance(HNMR)andcarbonnuclearmagnetic13resonance(CNMR)spectrawererecordedwithJEO
8、LAL-400(400MHz),JEOLECX-400(400MHz)orJEOLECA-500(500MHz)NMRspectrometers.Chemicalshiftsforprotonsarereportedin
