以八硝基苯基硅倍半氧烷（ONPS）为原料,5%Pd/C和FeCl3为催化剂,水合肼为还原剂,在四氢呋喃溶液中反应1h合成了八氨基苯基硅倍半氧烷（OAPS）.相比文献中已有的其它合成方法,该方法合成过程简单且稳定,催化效率高、产率高、周期短.通过FTIR,1HNMR,GPC对产物进行了表征,证明了硝基已完全转化.通过催化剂的控制,分离出ONPS向OAPS转化过程中的一种含有羟胺和二羟胺基团的中间体.分析了OAPS合成机理,提出了ONPS和水合肼的反应历程.认为ONPS中的硝基先经过2电子转移转化为二羟胺化合物,然后经过脱水加氢生成羟胺化合物,最后再经过脱水加氢生成OAPS;在有ONPS存在的情况下,水合肼主要转化为氮气和氢气,待ONPS完全转化为OAPS后,水合肼转化为氮气和氨气.%On the 5% Pd/C-FeCl3 catalyst,octa（aminophenyl）silsesquioxane（OAPS） was prepared in tetrahydrofuran（THF） using hydrazine hydrate as reductant from octa（nitrophenyl）silsesquioxane（ONPS） in 1 h.Compared with the synthesis methods in the references,this synthetic process was simple and stable,with shortened reaction period,increased yield and promoted catalytic efficiency.The product was characterized by FTIR,1H NMR and gel permeation chromatography（GPC） and it was found that nitro groups were com-pletely converted to amino groups.An intermediate with N,N-dihydroxyaminophenyl groups and hydroxyl-aminophenyl groups was obtained when the only 5% Pd/C was used as catalyst.The synthesis mechanism of OAPS from ONPS was studied based on the intermediate compound.In nitro groups reduction,N,N-dihydroxyaminophenyl groups were firstly formed through two-electron transfer,then hydroxylamino-phenyl groups were generated through dehydration/hydrogenation and finally aminophenyl groups were produced after further reduction.At the beginning,hydrazine hydrate was mainly oxidated to N2 and H2,but its oxidative products changed to N2 and NH3 when all of the ONPS were completely converted to OAPS.
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