作者:Stefan Scholz、Inge Sänger、Frauke Schödel、Michael Bolte、Hans-Wolfram Lerner
DOI:10.1016/j.inoche.2014.02.039
日期:2014.6
Abstract The reaction of PhSiCl 3 with one equivalent of Li[ t Bu] at r. t. yielded t BuPhSiCl 2 whereas t Bu 2 PhSiCl was only a minor product of the reaction of two molar equivalents Li[ t Bu] with PhSiCl 3 at 60 °C. By contrast, at r. t. t BuPhSiCl 2 was solely formed by this reaction. Treatment of PhSiCl 3 with three or more equivalents of Li[ t Bu] at 98 °C yielded a mixture of t Bu 2 PhSiH and
摘要 PhSiCl 3 与一当量 Li[ t Bu] 在室温下反应生成 t BuPhSiCl 2 而 t Bu 2 PhSiCl 只是两摩尔当量 Li[ t Bu] 与 PhSiCl 3 在 60 °C 反应的次要产物. 相比之下,在 rt t BuPhSiCl 2 仅由该反应形成。在 98°C 下用三当量或更多当量的 Li[tBu] 处理 PhSiCl 3 产生 t Bu 2 PhSiH 和 t Bu 2 (t BuC 6 H 4 CMe 2 CH 2 )SiH ( 3 ) 的混合物。两种硅烷可以很容易地彼此分离:从反应混合物中蒸馏出 Bu 2 PhSiH,并且可以从溶解的蒸馏残余物中结晶出硅烷 3。3 的 X 射线质量晶体在环境温度下从苯溶液中生长(单斜晶系,P 2 1 / c )。