邻苯二胺磷酰氯缩环氧丙醇酯的合成和表征

Synthesis and characterization of phosphate-glycidol O-diaminobenzene phosphoramidate(GDP)

采用邻苯二胺、三氯氧磷、环氧丙醇为原料合成一种新型磷酸酯类化合物邻苯二胺磷酰氯缩环氧丙醇酯(GDP).先以邻苯二胺、三氯氧磷为原料合成邻苯二胺磷酰氯(DP),再以DP、环氧丙醇为原料合成GDP,并用正交实验得到较好的反应条件.当邻苯二胺与三氯氧磷摩尔比为1∶1.3、反应时间为9 h、反应温度为82℃时,合成DP的产率达到88.6%;当DP与环氧丙醇摩尔比为1∶1、反应时间为24h、反应温度为30℃时,合成GDP的产率达到62.3%.分别测定了产物熔点并利用红外光谱仪、1H NMR对产物的结构进行了表征.

The new type phosphate, phosphate-glycidol O-diaminobenzene phosphoramidate （ GDP）, was synthesized by the 1,2-diaminobenzene, phosphorus oxychloride and glycidol. Using 1,2-diaminobenzene and phosphorus oxychloride as raw materials, O-phenylene diamine chloride（DP） was synthesized. Using DP and glycidol as raw materials, GDP was synthesized. Then the optimum synthetic process was obtained by orthogonal experimental design. The results showed that the optimum synthetic process was： in the first step, n（C6H8N2） ：n（POCl3） =1：1.3, reaction time 9 h, reaction temperature 82 ℃, the yield 88% ; in the second step, n（Dp） ：n（C3H6O2） = 1：1, reaction time 24 h, reaction temperature 30 ℃, the yield 62.3%. Chemical structure of the product was confirmed by IR,^1H NMR and melting point was measured.