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1、CatalyticCycloisomerizationontoaCarbonylOxygenShichengShi,†JonathanL.Kuo,†TaoChen†andJackR.Norton,††DepartmentofChemistry,ColumbiaUniversity,3000Broadway,NewYork,NewYork10027,UnitedStatesjrn11@columbia.eduSupplementaryInformationTableofContents1ExperimentalProceduresandCharacteri
2、zationData2•ReactionOptimization2•PreparationofStartingMaterials8•CycloisomerizationunderCobaloxime/H2condition17•Cycloisomerizationundersalen-Co(III)/silanecondition22•MechanisticStudies31References331Hand13CNMRSpectra34CorrespondingAuthor:Prof.Dr.J.NortonDepartmentofChemistryCo
3、lumbiaUniversity,3000BroadwayNewYork,NewYork10027,UnitedStatesE-mail:jrn11@columbia.eduAllstartingmaterialsreportedinthemanuscripthavebeenpreviouslydescribedinliteratureorpreparedbythemethodreportedpreviously.1-7Allexperimentsinvolvingcyclizationreactionwereperformedunderargoning
4、loveboxunlessstatedotherwise.AllsolventswerepurchasedatthehighestcommercialgradeandusedasreceivedorafterpurificationbypassingthroughactivatedaluminacolumnsordistillationfromNa/benzophenoneundernitrogen.Allsolventsweredeoxygenatedpriortouse.Allotherchemicalswerepurchasedatthehighe
5、stcommercialgradeandusedasreceived.Reactionglasswarewasoven-driedat140°Cforatleast24horflame-driedpriortouse,allowedtocoolundervacuum.Allproductswereidentifiedusing1HNMR,13CNMRand/orHR-MSanalysis.Allyieldsrefertoyieldsdeterminedby1HNMRusinganinternalstandard(nitromethane)unlessst
6、atedotherwise.1HNMRand13CNMRspectrawererecordedinCDCl3,CD2Cl2andAcetone-d6onBruker500Ascend,DRX500corDRX400spectrometer.Allcouplingconstants(J)arereportedinhertz(Hz).Abbreviationsare:s,singlet;d,doublet;t,triplet;q,quartet;brs,broadsinglet.High-resolutionmassspectra(HRMS)weremeas
7、uredona7TBrukerDaltonicsFT-MSinstrumentbyelectrosprayionization(ESI)probe.Allflashchromatographywasperformedusingsilicagel,60Å,300mesh.TLCanalysiswascarriedoutonglassplatescoatedwithsilicagel60F254,0.2mmthickness.Theplateswerevisualizedusinga254nmultravioletlamporaqueouspotassium
8、permanganatesolutions.1HNMR,13CNMRandHRM
