苯基亚膦酸二甲酯的合成

以苯、三氯化磷、甲醇为主要原料，经两步反应合成了苯基亚膦酸二甲酯，并通过正交实验优化了合成条件。第一步反应：苯和三氯化磷在三氯化铝催化剂作用下生成苯基二氯化膦，n（苯）：n（三氯化铝）：n（三氯化磷）=1：3：1．3，回流时间9h，三氯氧磷为处理剂，收率为95．5％。在第二步反应中苯基二氯化膦在三乙胺存在下与甲醇作用生成目的物，反应温度20～30％，优化的物料配比为n（苯基二氯化膦）：n（甲醇）：n（三乙胺）=1：2．2：2．7，在此条件下反应收率为88．4％。

Preparation of Dimethyl Phenyl Phosphonite

Dimethyl phenyl phosphonite had been synthesized from benzene,phosphorus trichloride and methanol in two steps.In the first step phenyl dichlorophosphine was prepared in 95.5% yield by reaction of benzene and phosphorous trichloride catalysted by aluminum trichloride.The optimum conditions were obtained as: n(C6H6)∶n(AlCl3):n(PCl3)=1∶3∶l.3,refluxing time 9 hours,and the product work-up with oxyphosphorus trichloride.In the second step dimethyl phenylphosphonite was prepared in 88.4% yield by reaction of phenyl dichlorophosphine and methanol at 20-30℃ in the presence of triethylaniline.The optimum molar ratio of reactants was n(phPCl2):n(CH3OH):nphN(CH3)2]=1∶2.2∶2.7.