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SHI Lan-xiang,ZHANG Bao-hua.One-pot synthesis of diethyl chlorophosphate[J].Journal of Hebei University of Science and Technology,2006,27(4):294-296
One-pot synthesis of diethyl chlorophosphate
Received:April 24, 2006  Revised:May 31, 2006
中文关键词:  氯磷酸二乙酯  亚磷酸二乙酯  一锅合成
英文关键词:diethyl chlorophosphate  diethyl phosphite  one-pot synthesis
Author NameAffiliation
SHI Lan-xiang College of Chemical Engineering, Shijiazhuang University, Shijiazhuang Hebei 050035,China 
ZHANG Bao-hua Department of Physics,Shijiazhuang University,Shijiazhuang Hebei 050035, China 
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      以三氯化磷、无水乙醇、四氯化碳为原料,一锅法合成氯磷酸二乙酯。四氯化碳既为原料又兼作溶剂,反应在无溶剂条件下进行,中间体亚磷酸二乙酯不经分离,直接与四氯化碳反应。对最佳原料配比、反应温度进行了优化,确定了三乙胺为最适宜的催化剂。当n(三氯化磷)∶n(无水乙醇)∶n(三乙胺)= 1∶(3.05~3.10)∶(0.10~0.12)、生成亚磷酸二乙酯阶段温度为50~60℃、生成氯磷酸二乙酯温度为25℃时,氯磷酸二乙酯的收率达72%。
      In one-pot synthesis of diethyl chlorophosphate (DCP) from phosphorus trichloride, anhydrous alcohol and carbon tetrachloride,carbon tetrachloride was used as material and solvent,and the intermediate diethyl phosphite was not isolated from the reaction mixture but directly reacted with carbon tetrachloride. The ratio of raw materials and reaction temperatures were investigated. Triethylamine as a catalyst was the most suitable. The optimal reaction condition:n(PCl3)∶n(EtOH)∶n(Et3N)= 1∶(3.05~3.10)∶(0.10~0.12), the reaction temperature were 50~60℃ (synthesis stage of diethyl phosphite), 25℃(synthesis stage of DCP). The yield of the product was 72%.
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