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以笼型低聚八苯基硅倍半氧烷(OPS)为原料,AlCl3为催化剂,苯磺酰氯为磺酰化试剂,在二氯甲烷溶液中反应72h,合成了笼型八(二苯砜基)硅倍半氧烷(ODPSS).该方法合成过程简单稳定,产率高.通过FTIR、MALDI-TOF MS、1H NMR、13C NMR、29Si NMR和元素分析对产物进行了表征,证明OPS已完全转化为ODPSS.通过改变溶剂、催化剂、反应时间和各反应物物质的量之比,优化了反应条件,分析了反应机理,建立了该体系下OPS的磺酰化反应机理模型.
Using cage oligomeric octaphenylsilsesquioxane (OPS) as raw material, AlCl3 as catalyst and benzenesulfonyl chloride as sulfonylating reagent, the reaction was carried out in dichloromethane solution for 72 h, (ODPSS) .The synthesis process is simple and stable with high yield.The product was characterized by FTIR, MALDI-TOF MS, 1H NMR, 13C NMR, 29Si NMR and elemental analysis to prove that OPS Completely transformed into ODPSS.The reaction conditions were optimized by changing the ratio of solvent, catalyst, reaction time and the amount of each reactant substance, the reaction mechanism was analyzed, and the mechanism model of sulfonylation of OPS was established.