CAJ | 학술논문

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 ，T HF）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、31 P 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％。
위강저삼（대갑기분기）련적합성성본，사합성과정록색화，이대갑기분기추화미위인발제，대록갑분、미설위원료，사경부남（Tetrahydrofuran ，T HF）위용제，합성격씨시제대갑기분기록화미。재이대갑기분록화미화삼록화린위원료，사경부남위용제，제비출목표산물삼（대갑기분기）련。산물경핵자（1 H NMR、31 P NMR）、질보측시표정여문헌일치。통과대량보반응적고찰，최가용제용량화적가온도위：매마이원료용제용량위350mL ，삼록화린적적가온도위0～10℃，재차공예조건하산솔가체도58％，차순도불소우98％。
In order to reduce the cost of tris (4‐methylphenyl) phosphine and make the synthesis process environmental ,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‐methyl‐phenyl) phosphine was prepared successfully ,and as characterized by 1 H NMR and 31 P NMR spectra .The results show that the best amount of solvent is 350mL per mol substance ,the op‐timal dropping temperature of phosphorus trichloride between 0~10℃ ,the highest yield 58% ,and the purity over 98%.