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题名: Synthesis of Aluminum Alkoxide and Bis-alkoxide Compounds Containing Bidentate Pyrrolyl Ligands
作者: Lin, Che-Yu;Lee, Hon-Man;Huang, Jui-Hsien
贡献者: 化學系
关键词: Aluminum;Alkoxides;Pyrrolyl
日期: 2007-08
上传时间: 2012-12-10T01:39:48Z
出版者: Elsevier
摘要: A series of aluminum alkoxide and bis-alkoxides compounds were synthesized and characterized. Reacting 1 with 1 and 2 equiv. of t-butanol in methylene chloride generates [C4H3N(CH2NMe2)-2]2Al(O-t-Bu) (2) and [C4H3N(CH2NMe2)-2-H-C4H3N(CH2NMe2)-2]Al(O-t-Bu)2 (3) in 47% and 54% yield, respectively. The 1H NMR spectrum of 2 exhibits two singlets for NMe2 and CH2N at δ 2.52 and 3.84, respectively, representing the symmetrical manner of molecular structure 2 in a solution. Compound 3 is not thermal stable in solution which decompose into substituted pyrrole ligand C4H4N(CH2NMe2)-2 and unknown aluminum alkoxides. Reacting 1 with 2 equiv. of triphenylsilanol in methylene chloride generates a tetra-coordinated aluminum “ate” compound [C4H3N(CH2NMe2)-2-H- C4H3N(CH2NMe2)-2]Al(OSiPh3)2 (4) in 49% yield. The 1H NMR spectra of 4 at room temperature show a broad signal at δ 1.57 for NMe2 fragments and the signals for CH2N were not observed. VT 1H NMR spectra of 4 show the NMe2 fragments became two singlets (δ 1.27 and 2.12) and the CH2N exhibited two doublets (δ 2.44 and 3.56) at 240 K. The fluxional energy barrier (ΔG‡) is estimated at ca. 50 kJ/mol. The molecular structures of compounds 3 and 4 are determined by single-crystal X-ray diffractometer.
關聯: Journal of Organometallic Chemistry, 692(17): 3718-3722
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