(Bis{2,4,6-triisopropylphenyl}stannylene)ferrocenophane and Related Ring-Opened Products
(Bis{2,4,6-triisopropylphenyl}stannylene)ferrocenophane and Related Ring-Opened Products
复制标题
(双{2,4,6-三异丙基苯基}亚锡基)二茂铁及相关开环产物
DOI：
10.1021/om9805234
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发表时间：
1999
期刊：
影响因子：
2.8
通讯作者：
K. Pannell
中科院分区：
文献类型：
--
作者：
H. Sharma;F. Cervantes;J. Mahmoud;K. Pannell
将二（2，4，6-三异丙基苯基）二氯化锡（1）加入到1，1 '-二硫代二茂铁-tmeda的己烷/THF浆液中，以良好的产率产生相应的甲锡亚基二茂铁烷（2）。2的结构分析显示两个环之间的二面角为14.7°，Fe−Sn原子距离相对较短，为2.994（2）A。2的循环伏安法表现出可逆的氧化还原行为。尽管用MeOH和H2O处理未能产生开环化合物，但硅胶催化的1的水解导致开环的Fc（i-Pr 3C 6 H2）2SnOH（3），其结晶为H-键合的二聚体。在180 °C下热处理2得到开环聚合产物4，其在从甲苯中沉淀后保持不溶于有机溶剂。4的固态13 C和119 Sn核磁共振谱证实了该材料的结构。报道了1的X射线结构分析，并与2进行了比较。
The addition of bis(2,4,6-triisopropylphenyl)tin dichloride (1) to a hexane/THF slurry of 1,1‘-dilithioferrocene−tmeda produces the corresponding stannyleneferrocenophane (2) in good yield. Structural analysis of 2 reveals a dihedral angle between the two cyclopentadienyl rings of 14.7° and a relatively short Fe−Sn atomic distance of 2.994(2) A. Cyclic voltammetry of 2 exhibits reversible redox behavior. Whereas treatment with MeOH and H2O failed to produce ring-opened compounds, silica gel catalyzed hydrolysis of 1 leads to ring-opened Fc(i-Pr3C6H2)2SnOH (3), which crystallizes as a H-bonded dimer. Thermal treatment of 2 at 180 °C leads to the ring-opened polymerization product 4, which after precipitation from toluene remains insoluble in organic solvents. Solid-state 13C and 119Sn NMR spectra of 4 confirm the structure of the material. The X-ray structural analysis of 1 is reported and compared to that of 2.