Synthesis of tetraphenylstannacyclopentadienes (stannoles). 1. Alkylation of 1,1-dihalostannoles leading to lithium 1,1-bis-(.eta.1-cyclopentadienyl)-1-halo-2,3,4,5-tetraphenylstannole, an [R4SnX]- anion, with pseudorotating axial- and equatorial-fluxional .eta.1-cyclopentadienyl groups
作者:W. A. Gustavson、L. M. Principe、W. Z. Min Rhee、J. J. Zuckerman
DOI:10.1021/ja00404a024
日期:1981.7
cleavage of hexaphenylstannole by elemental bromine and iodine, respectively, undergo conventional alkylation by methyllithium to form the expected 1,1-dimethylstannole, but treatment with excess lithium or thallium cyclopentadiene yields cubic crystals whose analytical data agree with the formulation X(C5H5)2SnC4(C4H5)4M where X=Br, M=Li, Tl and where X=I, M=Li. Infrared nu asym and nu sym (Sn-Br)
文摘: 1,1-二溴-和1,1-二碘-2,3,4,5-四苯基锡环戊二烯(二溴-和二碘锡醇)分别由元素溴和碘对六苯基锡的受控苯基锡裂解形成,通过甲基锂进行常规烷基化形成预期的 1,1-二甲基锡醇,但用过量的锂或环戊二烯铊处理产生立方晶体,其分析数据与公式 X(C5H5)2SnC4(C4H5)4M 一致,其中 X=Br、M=Li、Tl 和 X =I,M=Li。起始 dibromostannole 中的红外 nu asym 和 nu sym (Sn-Br) 吸收被 X=Br 产品中 225/cm 处的单个特征取代,3000 和 1595-695-695 cm(-1) 区域的吸收指定C5H5Sn 单元的 h(1)-环戊二烯性质。