摘要
以叔丁基二苯基氯硅烷(SCl)为原料,硼氢化钾/氯化锌(KBH_4/ZnCl_2)为还原体系,制备了叔丁基二苯基氢硅烷(SH),产物结构经~1H-NMR确证。通过单因素、正交实验和放大重复性实验确定了最佳反应条件为n(KBH_4)∶n(ZnCl_2)∶n(SCl)为2∶1.25∶1,100℃反应18h,平均收率为93.7%。该法具有原料易得,反应温和,操作方便,收率高,对环境友好等优点,适合工业化生产。
t-Butyldiphenylsilane(SH) was synthesized by t-butylchlorodiphenylsilane(SCl) in dioxane,using potassium borohydride/zinc chloride as the reduction system.The optimal conditions were selected as follows:n(KBH+4)∶n(ZnCl2)∶n(SCl)=2∶1.25∶1,reaction temperature was 100℃ for 18 h which were confirmed by orthogonal experimental design and repeated magnify experiments.The average yield was 93.7%.The structure of the product was investigated by 1H-NMR.The improved method was suitable for a scale production which was operation-convenient and environment-friendly.
出处
《化学研究与应用》
CSCD
北大核心
2017年第10期1569-1573,共5页
Chemical Research and Application