对苯二酚-二(4-氧代-4-磷杂-3,5,8-三氧杂双环[2.2.2]辛基)甲酸酯的合成及表征  

Synthesis and characterization of p-benzenediol-di(4-oxo-4-phospha-3,5,8-trioxobicyclo[2.2.2]octyl) formic ester

作　　者：高维英[1] 卢林刚[1] 于宝刚[1] 唐凯[1] 

机构地区：[1]中国人民武装警察部队学院科研部,河北廊坊065000

出　　处：《化学研究与应用》2009年第9期1327-1330,共4页Chemical Research and Application

基　　金："十一五"国家科技支撑计划资助项目(2006BAK06B06)

摘　　要：The pentaerythritol,phosphorus oxychloride,concentrated nitric acid,dichloro sulfoxide and hydroquinone etc.were used to synthesize a novel PEPA derivative with aryl:p-benzenediol-di(4-oxo-4-phospha-3,5,8-trioxobicycl[2.2.2]ooctyl)formic ester.The structure and thermal behaviors of the novel compound were identified and studied by FT-IR,1H NMR,ESI-MS and TGA respectively.The reaction conditions such as reaction temperature,solvent,material molar ratio etc.,were discussed.The suitable synthesis condition were defined as follows:reaction solvent was 1,4-dioxane,the molar ratio of the compound Ⅱ to the hydroquinone was 3∶1,reaction temperature was 101 ℃,reaction time was 3 h.Under the above conditions,the yield was 95.6%.The curves of TGA and DTG showed that the beginning temperature of decomposition of the compound was 295 ℃,the char content was 59% at 600 ℃,which had an excellent thermal stability and char forming.The pentaerythritol, phosphorus oxychloride, concentrated nitric acid, dichloro sulfoxide and hydroquinone ew. were used to synthesize a novel PEPA derivative with aryl ：p-benzenediol-di （4-oxo-4-phospha-3,5,8-trioxobicyclo [ 2. 2. 2 ] octyl） formic ester. The structure and thermal behaviors of the novel compound were identified and studied by FT-IR,＇ H NMR, ESI-MS and TGA respectively. The reaction conditions such as reaction temperature, solvent, material molar ratio etc. , were discussed. The suitable synthesis condition were defined as follows： reaction solvent was 1,4-dioxane, the molar ratio of the compound lI to the hydroquinone was 3：1 ,reaction temperature was 101 ℃ ,reaction time was 3 h. Under the above conditions,the yield was 95.6%. The curves of TGA and DTG showed that the beginning temperature of decomposition of the compound was 295 ℃, the char content was 59% at 600 ℃, which had an excellent thermal stability and char forming.

关 键 词：芳环 双环笼状磷酸酯 合成 表征 

分 类 号：O627.51[理学—有机化学]