苯基亚膦酸二乙酯的合成

Synthesis of Diethyl Phenylphosphonite

以苯、三氯化磷、乙醇为主要原料 ,经两步反应合成苯基亚膦酸二乙酯。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 (C6H6)∶n (PCl3 )∶n (AlCl3 ) =1∶3∶1.33,回流 12h ,三氯氧磷为处理剂 ,产率 88.6 %。第二步反应 :苯基二氯化膦在N ,N 二甲基苯胺存在下与乙醇作用生成目的物 ,n(phPCl2 )∶n (C2 H5OH)∶n [phN (CH3 ) 2 ]=1∶2 .5∶2 .2 ,反应温度 2 0— 30℃ ,产率 80 .4%。

The Diethyl phenylphosphonite has been synthesized by using benzene, phosphorus trichloride and ethyl alcohol as main raw materials by two-stage reaction. The first, phenyldichlorophosphine was prepared by the reaction of benzene and phosphorous trichloride in the presence of catalyst--aluminum trichloride, in the condition of n (C 6H 6)∶ n (PCl 3)∶ n (AlCl 3)=l∶3∶l.33, refluxing l2 hours, and treating the product by oxyphosphorus trichloride, the yield in first stage could reach 88.6%.The second, phenyl-dichlorophosphine reacts with ethyl alcohol at 20-30℃ in the presence of N,N-dimethylaniline to get the diethyl phenylphosphonite, and the yield of the stage was 80.4%.