季戊四醇螺环磷酰基二异丙醇的合成与表征

Synthesis and Characterization of the Spirocyclic Pentaerythritol Phosphodiisopropanol

以甲苯为溶剂,三乙胺为催化剂,以季戊四醇、三氯化磷、丙酮、甲酸等为原料,采用"一锅法"合成了季戊四醇螺环磷酰基二异丙醇,产率75%.以元素分析、IR、1HNMR、MS等手段表征了化合物结构,并以TGA、DSC表征了其热性能.结果表明,化合物初始分解温度大于200℃.质量分解50%时的温度为457℃,700℃后观察到残碳层为膨松的黑色固体,成炭量将近40%.同时以红外光谱、液相色谱等手段确定了主要副产物的结构.

With toluene as a solvent,triethy lamine as an activator,the phosphaspirocyclic compound 2,4,8,10-Tetraoxa-8,9-diphosphaspiro[5.5] undecane-3,9-dioxide-8,9-diisopropanol（DPDI） was prepared in a one-step reaction from the phosphorochloridite precursor with formic acid and acetone. Phosphorochloridite was synthesized through the reaction of pentaerythritol and phosphorus triehloride. The syntheses method is simple with total yield of 75%. The structures of compounds were characterized by IR,^1H NMR,MS and elemental analysis. The thermal stability of the product was analyzed with TGA and DSC. The initial decomposition temperature of DPDI is around 200℃, a 50℃ decomposition temperature was around 457℃, and the char yield is 40%. The byproduct was analyzed by IR and HPLC （High performance liquid chromatography）.