Lithium Aluminate Complexes and Alumoles from 1,4-Dilithio-1,3-Butadienes and AlEt2Cl

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• 作者：Yongliang Zhang ; Junnian Wei ; Wen-Xiong Zhang ; Zhenfeng Xi
• 刊名：Inorganic Chemistry
• 出版年：2015
• 出版时间：November 16, 2015
• 年：2015
• 卷：54
• 期：22
• 页码：10695-10700
• 全文大小：379K
• ISSN：1520-510X

文摘

A series of lithium aluminate complexes and alumoles were synthesized from 1,4-dilithio-1,3-butadienes 1 and AlEt₂Cl. Their structures were characterized using single-crystal X-ray structural analysis and NMR spectroscopy. The structure of the lithium aluminate complex 2-TMEDA showed that the Al atom adopted a tetra-coordinated mode bonded with two butadienyl C_sp2 atoms and two ethyl C_sp3 atoms. The lithium cation was located above the alumole ring. The structure of 3a revealed a dimeric 1-ethylalumole in the solid state. Diffusion ordered spectroscopy NMR spectra showed that 3a was also a dimer in C₆D₆ solvent. However, in tetrahydrofuran (THF) solution, the dimeric 3a dissociated into the 1-ethylalumole鈥揟HF adduct. The lithium aluminate complex 2 transformed into 3a-THF when treated with 1.0 equiv of AlEt₂Cl. Preliminary reaction chemistry and synthetic applications of the lithium aluminate complex were also investigated.