Attempted Isolation of Heavier Group 14 Element Ketone Analogues: Effect of O−H···π-Ar Hydrogen Bonding on Geometry
作者:Lihung Pu、Ned J. Hardman、Philip P. Power
DOI:10.1021/om010548u
日期:2001.11.1
the heavier group 14 element ketone analogues Ar2MO. Despite stringent precautions to exclude moisture and oxygen during the synthesis, the products 1 and 2 were isolated in ca. 30−50% yield. These results are in contrast to the recently reported stabilization of the terphenyl-protected, essentially strain-free, species (bisap)2GeO (bisap = 2,6-di(1‘-naphthyl)phenyl). Seemingly, 1 and 2 represent the
三联苯基14元素的宝石-二羟基(宝石-二醇)衍生物Ar 2 M(OH)2(Ar = C 6 H 3 -2,6-Mes 2 ; Mes = C 6 H 2 -2,4,6-Me 3),M = Ge(1); 合成了Sn(2),并通过X射线晶体学,NMR,IR光谱和燃烧分析对其进行了表征。合成途径涉及在烃溶液中用N 2 O或Me 3 NO处理二价MAr 2化合物。目的是分离较重的14族酮类似物Ar2 MO。尽管在合成过程中采取了严格的预防措施以排除水分和氧气,但产物1和2的分离度约为1。30-50%的收率。这些结果与最近报道的三联苯保护的,基本上无菌株的物种(bisap)2 GeO(bisap = 2,6-二(1'-萘基)苯基)的稳定化相反。看来1和2代表H 2 O加到Ar 2 MO中。其他产品的身份目前未知。化合物1代表锗宝石的第二个例子-二醇的结构特征,其特征在于预期的扭曲的四面体锗环境。化合