三(对甲基苯基)膦的合成与表征

The synthesis and characterization of tris(4-methylphenyl)phosphine

为降低三（对甲基苯基）膦的合成成本,使合成过程绿色化,以对甲基苯基溴化镁为引发剂,对氯甲苯、镁屑为原料,四氢呋喃（Tetrahydrofuran,THF）为溶剂,合成格氏试剂对甲基苯基氯化镁.再以对甲基苯氯化镁和三氯化磷为原料,四氢呋喃为溶剂,制备出目标产物三（对甲基苯基）膦.产物经核磁（1 H NMR、31P NMR）、质谱测试表征与文献一致.通过对两步反应的考察,最佳溶剂用量和滴加温度为：每摩尔原料溶剂用量为350mL,三氯化磷的滴加温度为0~10℃,在此工艺条件下产率可达到58%,且纯度不小于98%.

In order process envtronm to reduce the cost of tris（4-methylphenyl） phosphine and make the synthesis ental, using 4-methylphenyl magnesium bromide as initiator, p-chlorotoluene and magnesium as start material, and tetrahydrofuran as solvent, the grignard reagent 4-meth- ylphenyl magnesium chloride was synthesized. Then using 4-methylphenyl magnesium chloride and phosphorus trichloride as raw materials, and tetrahydrofuran as solvent, the tris（4-methylphenyl） phosphine was prepared successfully, and as characterized by 1H NMR and 31p NMR spectra. The results show that the best amount of solvent is 350mL per tool substance,the optimal dropping temperature of phosphorus trichloride between 0- 10℃, the highest yield 58 %, and the purity over 98 %.