一种新型有机磷酸季戊四醇二磷酸的合成

Synthesis of a new type of organic phosphate spirocy pentaerythritol diphosphate phosphoric acid

以三氯氧磷、季戊四醇为原料,首先合成螺环磷酸酯二酰氯,然后在螺环磷酸酯二酰氯的基础上合成季戊四醇二磷酸.主要介绍螺环磷酸酯二酰氯和季戊四醇二磷酸的合成工艺及改进方法,并用正交实验找出这两步反应的最优条件.当季戊四醇与三氯氧磷摩尔比为1∶8、温度为90℃、反应时间为10 h时合成的螺环磷酸酯二酰氯(SPDPC)的产率达79.98%.当SPDPC的浓度为0.033 7 mol·L-1、温度为20℃、反应时间为5 h时,合成的季戊四醇二磷酸(SPDPA)的产率达82.03%.同时,用熔点测试仪、红外光谱仪和1H NMR对产物的结构进行表征.

Using phosphorus oxychloride and pentaerythritol as initial materials, the spirocyclic pentaerythritol diphosphate phosphorus chloride （SPDPC） was synthesized and then the spirocy pentaerythritol diphosphate phosphoric acid （SPDPA） was synthesized on the base of SPDPC. The authors mainly discussed the improved synthesis technique of SPDPC and SPDPA in the paper. The optimum synthesis process was obtained by orthogonal experimental and the results showed that the optimum synthesis process was： for the first step, when n （pentaerythritol） ：n （phosphorus oxychloride） is 1：8, reaction temperature is 90 ~C, reaction time is 10 h, the yield is 79.98% ; tbr the second step, when the concentration of SPDPC is 0. 033 7 mol ~ L-1 , reaction temperature is 20 ~C, reaction time is 5 h, the yield is 82.03%. And the chemical structure of the products was confirmed by IR and 1H NMR.