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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Synthesis,structure and rectivity of ferrio-chloro-phosphnes,-arsanes and -stibanes[(CO)_2(mu~5-C_5Me_5)FePn(Cl)R](Pn=P,As,Sb);R=tetramethylcyclopentadienyl,2,7-di-tert-butyfluorenyl,2,7-di-tert-butyl-9-trimethylsilylfluorenyl)as precursor to novel m
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Synthesis,structure and rectivity of ferrio-chloro-phosphnes,-arsanes and -stibanes[(CO)_2(mu~5-C_5Me_5)FePn(Cl)R](Pn=P,As,Sb);R=tetramethylcyclopentadienyl,2,7-di-tert-butyfluorenyl,2,7-di-tert-butyl-9-trimethylsilylfluorenyl)as precursor to novel m

机译:亚铁-氯膦,ar烷和-stibanes [(CO)_2(mu〜5-C_5Me_5)FePn(Cl)R](Pn = P,As,Sb); R =四甲基环戊二烯基,2的合成,结构和定性,7-二叔丁基芴基,2,7-二叔丁基-9-三甲基甲硅烷基芴基)

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摘要

Reaction o fone equivalent of the complexes[FeCp~*(CO)_2PnCl_2](Pn=P,As,Sb)with tetramethylcyclopentadienyl-lithium afforded compouns[FeCp~*(CO)2{Pn(Cl)(C_5Me_4H}].dehydrochlorination by means of tert-butyllithium led to decomposition.Only in the case of the phosphorus ocmpound was evidence for the initial formation of a phosphaalkene given by ~(31)P NMR spectroscopy.Similarly treatment of equimolar amounts of [FeCp~*(CO)_2PnCl_2]with2,7-di-tert-butyl-9-H-fluorenyllithium or 2,7-di-tert-butyl-9-trimethylsilyfluorenyllitium yielded the asymmetrically substituted feriopnicogenanes [FeCp~*(CO)_2{Pn(Cl)-9-R-Fl~*}] (Pn=P,As,Sb;R=H,Me_3Si;Fl~*=2,7-di-tert-butylfluorenylidene).Dehydrohalogenation of [FeCp~*(CO)_2{Pn(Cl)-9-H-Fl~*}] with lithium diisopropylamide resulte din the formation of the anticipated phosphaalkene[FeCp~*(CO)_2{Pn(9-H-Fl~*)_2}](Pn=As,Sb)wre obtained as products.The new compounds were characterized by elemental analyses and spectra (IR,~1H,~(13)C,~(29)Si,~(31)P NMR).The molecular structures of [FeCp~*(CO)2{Pn(Cl)(C_5Me_4H}](Pn=As,Sb),[FeCp~*(CO)2{As(Cl)-(9-Me_3Si-Fl~*)}] and [FeCp~*(CO)2{Sb(9-H-Fl~*}_2] were elucidated by single X-ray diffraction analyses.
机译:等价的配合物[FeCp〜*(CO)_2PnCl_2](Pn = P,As,Sb)与四甲基环戊二烯基锂反应,得到化合物[FeCp〜*(CO)2 {Pn(Cl)(C_5Me_4H}]。脱氯化氢〜(31)P NMR光谱分析表明,只有在磷化合物存在的情况下,磷的存在才可以初步形成磷烯烃。同样处理等摩尔量的[FeCp〜*(CO)带有2,7-二叔丁基-9-H-芴基锂或2,7-二叔丁基-9-三甲基硅芴基锂的_2PnCl_2]产生不对称取代的硫杂环庚烷[FeCp〜*(CO)_2 {Pn(Cl)- 9-R-Fl〜*}](Pn = P,As,Sb; R = H,Me_3Si; Fl〜* = 2,7-二叔丁基芴叉)。[FeCp〜*(CO)_2 { Pn(Cl)-9-H-Fl〜*}]和二异丙基氨基锂导致形成预期的磷烯烃[FeCp〜*(CO)_2 {Pn(9-H-Fl〜*)_ 2}](Pn =将其作为产物获得。通过元素分析和光谱(IR,〜1H,〜(13)C,〜(29)Si,〜(31)P NMR)对新化合物进行表征。 [FeCp〜*(CO)2 {Pn(Cl)(C_5Me_4H}](Pn = As,Sb),[FeCp〜*(CO)2 {As(Cl)-(9-Me_3Si-Fl〜*) }}]和[FeCp〜*(CO)2 {Sb(9-H-Fl〜*} _ 2)]进行了单次X射线衍射分析。

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