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Synthesis, Structure And Catalytic Activity Of Organolanthanide Complexes With N-piperidineethyl Substitued Indenyl Ligands

Posted on:2006-10-12Degree:MasterType:Thesis
Country:ChinaCandidate:X L TangFull Text:PDF
GTID:2121360155450975Subject:Organic Chemistry
Abstract/Summary:PDF Full Text Request
All experiments were carried out under the dry and oxygen-free argon atmosphere by using standard Schlenk techniques. Reaction of C1CH2CH2NC5H10 with 1 equiv of C9H7Li in THF at 0℃ yielded C9H7CH2CH2NC5H10(1) in 61% yield, 1 reacted with 1 equiv of n-BuLi in THF at 0℃ yielded C5H10NCH2CH2C9H6Li, interaction of C5H10N -CH2CH2C9H6Li with excess Me3SiCl yielded C9H6-1-Me3Si-3-CH2CH2NC5H10(2) in 75% yield.Interaction between [(Me3Si)2N]3Yb~III(u-Cl)Li(THF)3 and 2 equiv of 1 in refluxed toluene for 24 hours, after recrystallization from toluene, gave an ytterbium(II) complex [ η~5: η1-C9H6CH2CH2NC5H10]2Yb~II (3) in 67% yield. Treatment of [(Me3Si)2N]3Yb~III(μ-Cl)Li(THF)3 with 2 equiv of 2 in toluene at 80℃, after recrystallization from n-hexane, gave an ytterbium(II) complex [ η4: η2: η1-(C5H10NCH2CH2C9H5SiMe3)Li(μ-Cl)] Yb( η5: η1-C5H10NCH2CH2C9H5SiMe3) (4) in 54% yield. Interaction of [(Me3Si)2N]3Eu~III(μ-Cl)Li(THF)3 with 2 equiv of 1 in toluene at 50℃ for 24 hours, gave a europium (II) complex [ η5: η1-C9H6CH2CH2N C5H10]2Eu~II-LiCl(5) in 75% yield. Treatment of [(Me3Si)2N]3Eu~III( μ -Cl)Li (THF)3 with 2 equiv of 2 in toluene at 50℃, after recrystallization from toluene, gave a europium (II) complex [ η5: η1-C9H5-1-Me3Si-3 -CH2CH2NC5H10]2Eu~II.LiCl (6) in 50% yield. Interaction of [(Me3Si)2N]3 Sm~III( μ-Cl)Li(THF)3 with 2 equiv of 1 in toluene at 80℃ for 24 hours, after recrystallization from toluene, gave a samarium(III) complex [ η4: η3: η3: η1-C9H6CH2CH2NC5H10]3Sm~III (7) in 72% yield. Treatment of [(Me3Si)2N]3Nd~III(μ-Cl)Li(THF)3 with 2 equiv of 1 in toluene at 80℃ for 24 hours, after recrystallization from toluene, gave a neodymium(III) complex [ η4: η3: η3: η1-C9H6CH2CH2NC5H10]3Nd~III(8) in 62% yield. Interaction of [(Me3Si)2N]3Sm~III( μ-Cl)Li(THF)3 with 2 equiv of 2 in...
Keywords/Search Tags:organolanthanide complexes, synthesis, ligand, homolysis, catalysis, polymerization
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