Synthesis, electrochemical behavior and EPR study of organometallic [5]trovacenylthiol (畏⁷-C₇H₇)V(畏⁵-C₅H₄SH) and structural characterization of ansa-trithio[3]trovacenophane

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• 作者：Christoph Elschenbroich ; Feng Lu ; Klaus Harms ; Olaf Burghaus
• 关键词：Electrochemistry ; Electron paramagnetic resonance ; Organometallic thiol ; Sulfide
• 刊名：Journal of Organometallic Chemistry
• 出版年：1 April, 2014
• 年：2014
• 卷：755
• 期：Complete
• 页码：58-63
• 全文大小：720 K

文摘

Organometallic paramagnetic [5]trovacenylthiol (3) was prepared by acidification of lithium [5]trovacenylthiolate 2, which was synthesized via elemental sulfur oxidative insertion to C-Li bond of [5]trovacenyllithium. [5]Trovacenylthiol (3) was investigated by means of cyclic voltammetry and electron paramagnetic resonance (EPR). However, the reaction of concentrated DME solution of 2 with S₂Cl₂ unprecedentedly afforded ansa-trithio[3]trovacenophane (6), which was demonstrated by X-ray diffraction analysis. Furthermore, three efficient strategies have been explored to construct S-C, S-Si bond of organometallic alkyl, aryl [5]trovacenyl sulfides (7, 8, 9) and silylthioester (10) in the absence of transition-metal catalyst under mild reaction conditions.