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三氯单茂(茚)锆络合物的合成一直以来都是一个难点,往往伴有双茂(茚)锆络合物的产生.本工作通过侧链吡啶取代的茚基的锂盐直接与ZrCl4?2THF反应选择性的生成了一类具有螯合环状结构的半夹心三氯一茚锆络合物[Ind-Bridge-Py]ZrCl3?THFx(CN1~CN3),无双茚锆络合物的生成.与传统单茚锆络合物的合成方法相比,此类吡啶茚锆络合物的合成方法具有操作简单,产物单一且较易分离,产率较高等优点.CN2[Bridge:C(Me,Et)CH2]单晶证明侧链吡啶的N原子与锆配位,同时络合物晶体中含有两分子四氢呋喃,一分子四氢呋喃中的氧与锆配位,而另一分子则呈游离状态.
The synthesis of trichloro-monocenes (indene) zirconium complexes has always been a challenge, often accompanied by the production of bis-metallocene (indene) zirconium complexes.In this work, the side-chain pyridine-substituted indenyl lithium salts were directly reacted with ZrCl4? 2THF reaction selectively generated a class of semi-sandwich trichloro-indene zirconium complexes [Ind-Bridge-Py] ZrCl3? THFx (CN1 ~ CN3) .Compared with the synthesis of the traditional single indene zirconium complex, the synthesis method of the pyridine indene zirconium complex has the advantages of simple operation, single product and easy separation, high yield, etc. CN2 [Bridge: C (Me, Et) CH2] shows that the N atom of the side-chain pyridine is coordinated with zirconium. At the same time, the complex crystal contains two molecules of tetrahydrofuran, one of the oxygen in the molecule of tetrahydrofuran is coordinated with zirconium, and the other molecule is free status.