5H-苯基联苯膦磺化产物中氧化组分的结构鉴定  

Structure Determination of the Oxidation Components in Phenyldibenzophosphole Sulfonated Products

作　　者：董慧茹[1] 张敬畅[1] 张建军[1] 金花[1] 

机构地区：[1]北京化工大学应用化学系,北京100029

出　　处：《分析化学》2002年第8期990-993,共4页Chinese Journal of Analytical Chemistry

基　　金：国家科委"九五"科技攻关项目 ( 96A12 0 4 0 5)

摘　　要：用薄层色谱法制备了 5H 苯基联苯膦磺化产物中氧化组分 ,即A斑和B斑的纯品 ;分别用电喷雾质谱 (ESI MS)、1 3C和1 H核磁共振波谱 (1 3C NMR ,1 H NMR)及红外光谱法 (IR)鉴定其结构。经ESI MS、1 3C NMR、1 H NMR和IR谱的解析 ,发现 4种谱图相互对应 ,证明了A斑和B斑组分分别为二磺化和三磺化苯基联苯膦的氧化物 。Thin layer chromatography (TLC) was applied to separate phenyldibenzophosphole (PDBP) sulfonated products, and the structure of PDBP oxides in PDBP sulfonated products was determined by electrospray ionization-mass spectrometry (ESI-MS), C-13-nuclear magnetic resonance (NMR), H-1-NMR and infrared spectroscopy (IR). Through a series of experiments, the TLC optimum conditions were silica gel 60 F-254 as absorbent, isopropanol: ethanol: ammonium = 1 : 1 : 1 as mobile phase, activation at 105 degreesC for about 50 min. The spots are located by ultraviolet (UV) light (lambda = 254 nm). The PDBP sulfonated products usually can be separated into four to six spots. The pure substances of A spot and B spot were prepared by TLC, and their structures were determined by electrospray ionization-MS, C-13-NMR, H-1-NMR and IR, the results showed they were disulfonated and trisulfonated PDBP oxides.

关 键 词：氧化组分 结构鉴定 薄层色谱 质谱 红外光谱 核磁共振波谱 5H-苯基联苯膦磺化产物 

分 类 号：O658[理学—分析化学]