Selective Preparation of Sterically Encumbered Diaryltin Dihalides from Grignard Reagents via Salt Metathesis and Halide Exchange
作者:Beate G. Steller、Roland C. Fischer
DOI:10.1002/ejic.201900180
日期:2019.6.10
A general route for the selective preparation of diaryltin dichlorides, dibromides, and diiodides from readily accessible but sterically demanding, 2,6‐disubstituted or 2,4,6‐trisubstituted aryl Grignard reagents ArylMgBr and tin tetrachloride was developed. During work‐up, the initially obtained mixture of halides is converted into a single species. The thus obtained diaryltin dichlorides were reacted
[Cr(eta(5)-C5H4Li)(eta(7)-C7H6Li)]2 x (thf)8, where the C5H4 moieties of both units are connected by two bridging lithium atoms. Addition of different element dihalides to the dilithio precursor facilitated the isolation of ansa complexes with boron and germanium in the bridging position. Structural characterization by X-ray diffraction studies on [Cr(eta(5)-C5H4)-BN(SiMe3)2-(eta(7)-C7H6)] and [Cr(eta(5)-C
杂配夹心复合物 [Cr(eta(5)-C5H5)(eta(7)-C7H7)](三氯苯)是通过随后在环庚三烯存在下用 NaCp 和 Mg 处理 CrCl3 制备的,产率为 40%。采用 tBuLi/tmeda(N、N、N'、N'-四甲基乙二胺)的选择性二金属化提供了高活性物质 [Cr(eta(5)-C5H4Li)(eta(7)-C7H6Li)] x tmeda。对其 thf 溶剂化物的 X 射线晶体结构测定揭示了固态的对称二聚体组成,即 [Cr(eta(5)-C5H4Li)(eta(7)-C7H6Li)]2 x (thf)8,其中两个单元的 C5H4 部分由两个桥接锂原子连接。向二锂前体中添加不同的二卤化物元素促进了在桥接位置具有硼和锗的 ansa 复合物的分离。通过 X 射线衍射研究 [Cr(eta(5)-C5H4)-BN(SiMe3)2-(eta(7)-C7H6)] 和 [Cr(eta(5)-C5H4)-GeMe2-(
Synthesis and Reactivity of [2]Ferrocenophanes with C−Ge and C−Sn Bridges
作者:Alexandra Bartole-Scott、Rui Resendes、Frieder Jäkle、Alan J. Lough、Ian Manners
DOI:10.1021/om049650s
日期:2004.12.1
Ph, Me or E = Sn, R = tBu, Mes, Me) and were characterized by 1H, 13C, and 119Sn NMR, UV/vis, MS, and in representative cases elemental analysis. X-ray diffraction analysis of these species revealed structures possessing moderate ring-tilt with values in the range α = 10.99(2)−11.81(5)° for 11a,b and α = 6.64(2)−7.5(1)° for 12a−c. The presence of a small or moderate degree of ring-strain was further
的合成,表征,和新颖carbogerma的反应[2] ferrocenophanes,(η-C 5我4)的Fe(η-C 5 H ^ 4)CH 2 GER 2,11(一,R = Ph值; b,R =我),以及carbostanna [2] ferrocenophanes,(η-C 5我4)的Fe(η-C 5 H ^ 4)CH 2 SNR 2,12(一,R =吨卜; b,R =的Mes; C ^,R =我)。化合物11a,b和图12A - ç,分离从反应橙色晶体(η-C 5我4)的Fe(η-C 5 H ^ 4 Li)的CH 2李· X TMEDA有Cl 2 ER 2(E =锗,R =苯基,Me或E = Sn,R = t Bu,Mes,Me),并通过1 H,13 C和119 Sn NMR,UV / vis,MS进行表征,并在代表性情况下进行元素分析。对这些物种的X射线衍射分析表明,对于11a和b,这些结构具有适度的环倾角,其值在α=
1,3,2,4-Diselenastannaboretane, a novel selenium-containing four-membered boracycle: synthesis, structure and thermal cycloreversion into a selenoxoborane
作者:Mitsuhiro Ito、Norihiro Tokitoh、Renji Okazaki
DOI:10.1039/a806478d
日期:——
Treatment of an overcrowded aryl trihydroborate bearing 2,4,6-tris[bis(trimethylsilyl)methyl]phenyl (Tbt) group with Cp2TiSe5 followed by the addition of Ar2SnCl2 (Ar = Ph or Mes) and Ph3P resulted in the isolation of novel selenium-containing four-membered boracycles, 1,3,2,4-diselenastannaboretanes, the thermolysis of which in the presence of 2,3-dimethyl-1,3-butadiene or 2,4,6-tri-tert-butylbenzonitrile oxide indicated the formation of a novel class of boron-containing doubly bonded compound, an arylselenoxoborane (Tbt)BSe.