双(4-氟苯基)-3′-二乙氧基膦酰苯基氧膦的合成与表征

Synthesis and characterization of bis(4-fluorinated phenyl)-3′-diethoxyl phosphonyl phenyl phosphine oxide

在氮气保护系统中,将双（4-氟苯基）-3 ＇-碘苯基氧膦、Pd（PPh3）4、三乙胺和亚磷酸二乙酯溶解在甲苯中,加热到80℃,反应过夜（TLC监测反应）.反应完成后经色谱柱层析分离（200～300目,石油醚/乙酸乙酯）,得到双（4-氟苯基）-3＇-二乙氧基膦酰苯基氧膦,纯度高于99.5％.采用核磁共振、熔点仪及HRMS（ESI）等方法对产物的结构进行表征,结果表明合成的化合物结构与理论结构一致.

Under a nitrogen atmosphere, bis （4-fluorinated phenyl）-3＇-iodophenyl phosphine oxide, Pd （PPh3）4, triethylamine and phosphate ester were dissolved in toluene, then heated to 80 ℃. The mixture was stirred for one night and monitored by TLC analysis. After the completion of the reaction, the solution was concentrated and purified by column chromatography（200-300 mesh, gradient eluted with petroleum ether/ethyl acetate） to yield the expected bis（d-fluorinated phenyl）-3＇-diethoxyl phosphonyl phenyl phosphine oxide. The purity of the product is higher than 99.5%. The structure of the product synthesized was demonstrated to be consistent with the theoretical structure by NMR, melting point measurement and HRMS （ESI）.