氯代二异丙基膦合成工艺的研究

Study on the Synthesis of Chlorodiisopropylphosphine

介绍了以镁、氯代异丙烷和三氯化膦为主要原料,四氢呋喃为溶剂合成氯代二异丙基膦的方法。研究得到了该反应的最佳反应条件为:n(PCl3):n(i-C3H7MgCl)=1:1.8;反应温度:-30^-35℃;滴加时间1.25h[n(PCl3)=0.154mol;n(i-C3H7MgCl)=0.278mol]。四氢呋喃代替乙醚作为溶剂,加速了反应的进行,将氯代二异丙基膦的产率提高至71.64%。该条件下合成氯代二异丙基膦,得到澄清的溶液,反应生成的氯化镁容易处理,减小了反应对环境污染,属于清洁生产。

A method of synthesizing chlorodiisopropylphosphine,in which the raw are magnesium,isopropyl chlorides and phosphorus trichloride,the solvent is tetrahydrofuran,is introduced in this paper.The optimal reaction conditions are as follows:n(PCl3):n(i-C3H7MgCl)=1:1.8;-30℃～-35℃;1.25 hour[n(PCl3)=0.154mol;n(i-C3H7MgCl)=0.278mol].That using the tetrahydrofuran instead of ether as the solvent improved the safety and the yield of the reaction.The yield is up to 71.64%.Another improvement is that the solution received in the synthesis is clear,and it is easy to treat with the residue comparing with other conditions.It is a cleaner production.