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Synthesis and Characterisation of Two Lithium Tetramethylberyllate Salts and a Series of β-Diketiminato Beryllium Alkyl Complexes
Australian Journal of Chemistry ( IF 1.0 ) Pub Date : 2020-06-19 , DOI: 10.1071/ch20129
Albert Paparo , Caspar N. de Bruin-Dickason , Cameron Jones

A safer route than that previously published for the synthesis of [BeI2(OEt2)2] has been developed. Reactions of beryllium dihalide complexes [BeX2(OEt2)2] (X = Br or I) with either LiMe or LiBun lead to mixtures of products, which have been shown to act as sources of ‘BeR2’ (R = Me or Bun) in previous synthetic studies. Here, a titration method has been developed to determine the quantity of metal alkyl residues in these ‘BeR2’ mixtures that are available for subsequent alkane elimination reactions. Treating ‘BeMe2’ mixtures with N,N,N′,N′-tetramethylethylenediamine (tmeda) gave two lithium tetramethylberyllate compounds, [{(tmeda)Li}2(μ-BeMe4)] and [{[(tmeda)Li](BeMe4)(μ-Li)}], which were crystallographically characterised. Treatment of in situ-generated ‘BeR2’ solutions with several β-diketimines (HC{C(Me)=NR}{=C(Me)N(H)R}, NacnacH, R = aryl or alkyl) yielded a series of β-diketiminato beryllium alkyl complexes, [(Nacnac)BeR], including the first chiral example of such a compound. Crystallographic studies of these reveal them to be monomeric, with planar three-coordinate beryllium centres.



中文翻译:

两种四甲基铍酸锂盐和一系列β-二酮亚胺基铍烷基络合物的合成与表征

已经开发出比先前公开的[BeI 2(OEt 22 ]的合成更安全的途径。的铍二卤化物配合物[BEX反应2(OET 22 ]与任一石灰或礼部(X = Br或I)ñ导致的产品,这已被证明作为“BER的来源的混合物2 ”(R =我或Bu n)。在这里,已经开发出一种滴定方法来确定这些“ BeR 2 ”混合物中可用于后续烷烃消除反应的金属烷基残基的数量。用N处理'BeMe 2 '混合物ÑN' Ñ 'N'-四甲基乙二胺(TMEDA),得到两个锂tetramethylberyllate化合物,[{(TMEDA)栗} 2(μ-BEME 4)]和[{[(TMEDA)栗(BEME 4)(μ- Li)} ],通过晶体学表征。用几种β-二酮亚胺(HC {C(Me)= NR} {= C(Me)N(H)R},NacnacH,R =芳基或烷基)处理原位生成的'BeR 2 '溶液产生了一系列β-二酮基亚甲基铍烷基配合物[(Nacnac)BeR]的合成,包括该化合物的第一个手性实例。这些晶体的晶体学研究表明它们是单体的,具有平面的三坐标铍中心。

更新日期:2020-08-20
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