二羰基[三-(三甲硅基)]环戊二烯基铁卤化物的合成及结构  

Syntheses and Structures of Dicarbonyl Tris(Trimethylsilyl)-cyclopentadienyl Iron Halides

作　　者：孔垂华[1] 徐善生[1] 周秀中[1] 王如骥[2] 王宏根[2] 

机构地区：[1]南开大学元素有机化学实验室 [2]南开大学中心实验室,天津300071

出　　处：《有机化学》1995年第3期312-317,共6页Chinese Journal of Organic Chemistry

基　　金：国家自然科学基金;教委博士学科点基金

摘　　要：三-(三甲硅基)环戊二烯与五羰基铁在二甲苯中回流6h,反应停留在生成η_5-[Me_3Si)_3C_5H_2]Fe(CO)_2H(1)的中间阶段,这是由于茂环上有三个大位阻取代基(Me_3Si)的存在阻止了1进一步反应成双核Fe—Fe键化合物。1分别与CHCl_3·NBS及I_2反应,生成相应的铁卤化物,η_5-[1,2,4-(Me_3Si)_3C_5H_2]Fe(CO)_2X(X:Cl,2;Br,3;I,4)。测定了2的晶体结构,晶体属单斜晶系,C_c空间群,晶胞参数α=9.856(4),b=20.230(5),c=11.717(9);β=92.38(5)°,V=2334(3)~3,Z=4,D=1.22g·cm^(-3)。The xylene solution of tris (trimethylsilyl) cyclopentadiene and Fe(CO)5 was refluxed for 6h. The reaction was stopped at intermediate step of formation of the corresponding mononuclear iron hydride η-[(Me3SiC5H2] Fe(CO)2H (1). 1 cannot proceed further to form the dinuclear(Fe-Fe) product. It is probably due to the steric effect of three silyl groups on Cp-ring which hindered the further progress of the reaction. 1 reacted respectively with CHCl3, NBS and iodine to afford the corresponding iron halides η-[ 1,2, 4-(Me3SiC5H2)] Fe(CO)2X (X: Cl, 2; Br, 3; I, 4). The crystal structure of 2 was determined by X-ray crystallography. The crystal is monoclinic, space group Cc with a = 9.856(4), b = 20.230(5), c=11.717(9)A; β = 92.38(5)° , v=2334(3)A3, z = 4, Z)c=1.22g · cm-3.

关 键 词：三甲硅基 环戊二烯 合成 晶体结构 铁卤化物 

分 类 号：O627.81[理学—有机化学]