高效合成含P—O—P键化合物:焦膦酸酯、四烷基焦膦酸酯和焦膦酰胺的方法

Development of an Efficient Method for the Synthesis of Compounds Containing P—O—P Bonds:Pyrophosphonates,Tetraalkyl Pyrophosphates and Pyrophosphonamidates

研究了焦膦酸酯、四烷基焦膦酸酯和焦膦酰胺的合成方法.原料烷基氯膦酸酯、Et_(3)N和水以1∶1.2∶0.5(物质的量比)的比例,丙酮为溶剂,回流条件下,反应15 min,焦膦酸酯的产率最高可达95%.以三乙胺为反应溶剂及缚酸剂的方法合成四烷基焦膦酸酯和焦膦酰胺的速率和产率较使用传统方法更加高效.

This work describes a method of synthesizing pyrophosphonates,tetraalkyl pyrophosphates and pyrophosphonamidates.Pyrophosphonates can be synthesized by the reaction of alkyl dichlorophosphonate,triethylamine(Et_(3)N),and water,in a molar ratio of 1∶1.2∶0.5(dichlorophosphonate∶Et_(3)N∶water).When the reaction was allowed to proceed for 15 min in acetone,the maximum yield recorded for the pyrophosphonates was 95%.Et_(3)N was the solvent,with an acid-binding agent.Following this method,the achieved rate of production of tetraalkyl pyrophosphate and pyrophosphonamidate was faster than the rate of production of the compounds reached using traditional methods.