摘 要 本論文中實驗可以分成兩個部分：第一部分是改良原始文獻中合成立方體結構之矽氧烷類化合物(cubic silsesquioxanes)的方法。以三乙氧基苯矽烷(phenyltriethoxysilane)為原料，在使用苯(benzene)、氰甲烷(acetonitrile)、甲苯(Toluene)為溶劑下，於不同反應條件下合成六面體苯矽氧烷[octaphenylsilsesquioxane，以下簡稱為OPS， ]，比較時間與其相對產率，改善原本OPS之合成耗時的缺點。再將OPS以混酸進行硝化反應合成六面體硝基苯矽氧烷[octa(nitrophenyl)silsesquioxane，以下簡稱為ONPS， ]，取代文獻中不易取得的高濃度發煙硝酸。再將ONPS嘗試以聯胺與鈀/活性碳的方法還原成胺基苯矽氧烷[octa(amino- phenyl)silsesquioxane，以下簡稱為OAPS， ]，與文獻中之還原方法比較還原效果及後處理之優缺點。 第二部分：以OAPS為顯色劑(developing agent)，以鹽酸與亞硝酸鈉使之重氮化，與不同基劑(ground；如：β- Abstract This master's thesis can be mainly described in two parts. Part.1: The synthesis of octaphenylsilsesquioxane(OPS) under different reaction conditions by using phenyltriethoxysilane as a reactant in aprotic solvents,such as benzene , acetone -trile , toluene.The synthesis is compared with the original approach published earlier by reaction time and its corres -ponding yields to improve the disvantage of taking too much time.Then, Octa(nitrophenyl)silsesquioxane (ONPS) is prepared by nitration of OPS in the mixture of nitric acid and sulfuric acid instead of the unavailable highly concentrated fuming nitric acid. ONPS is transformed to OAPS by the reduction method of hydrazine and Palladium on active carbon as the catalyst,and make a comparison between the different reduction method. Part.2:Using OAPS,diazotized by adding hydrochlorric acid and sodium nitrite ,as a developing agent couple with different grounds(β-naphthol ,G-acid ,H-acid ,etc.) to form kinds of azoic dyes. The monographs about OAPS which have been published is to form the polyimide complex with excellent thermal stability,but there are no researches about azoic dyes. As OAPS has a property of one anino group on each benzene ring ,it appears to provide a good building block for the construction of materials.Using the propertity to synthesize diazo dyes,expecting the resulting products has 8 chromogens in one molecular to improve the dying ability.