二(邻-三氟甲基苯基)二硫代次膦酸的合成  

Synthesis of Bis-(o-Trifluoromethylphenyl) Dithiophosphinic Acid

作　　者：王红敏[1,2] 贾彩[2] 文明芬[2] 李保山[1] 陈靖[2] 

机构地区：[1]北京化工大学化工资源有效利用国家重点实验室,北京100029 [2]清华大学核能与新能源技术研究院,北京102201

出　　处：《核化学与放射化学》2010年第5期280-282,共3页Journal of Nuclear and Radiochemistry

基　　金：国家自然科学基金资助项目(No.20702028)

摘　　要：在合成系列二硫代次膦酸的研究中,对二(邻-三氟甲基苯基)二硫代次膦酸的合成方法进行了改进。以三氯化磷(PCl3)和邻-三氟甲基苯基溴化镁((o-F3CC6H4)MgBr)为原料,经格氏反应、硫化以及硫氢化钠取代等三步连续进行的反应合成得到了产品。所得产品FTIR谱图显示有取代苯环、C—F键、P—S单键和P S双键的特征吸收峰,经31P NMR、1H NMR和13C NMR谱图解析和质谱分析结果表明,所得产物结构与目标产物二(邻-三氟甲基苯基)二硫代次膦酸结构完全符合。The synthetic method of bis-（o-trifluoromethylphenyl）dithiophosphinic acid has been improved during the synthetic research of various dithiophosphinic acids.The optimized synthesis has been realized with PCl3 and（o-F3CC6H4）MgBr as starting materials and via a continuous three-step method including Grignard reaction,sulfuration and substitution reaction.The FTIR spectrum of product shows the presence of substituted aromatic ring,C-F bond,P-S single bond and P=S double bond.The interpretation result of 31P NMR,1H NMR and 13C NMR of the product,as well as MS,is completely in line with the structure of the targeted compound bis-（o-trifluoromethylphenyl）dithiophosphinic acid.

关 键 词：二硫代次膦酸 合成 萃取剂 

分 类 号：O625.1[理学—有机化学]