磷酸苯基二乙基酯的合成及NMR和ESI-MS/MS测定  

THE PHOSPHORYLATION REACTION STUDIED BY NMR AND ESI-MS/MS

作　　者：陈晓岚[1] 廖新成[1] 卢建莎[1] 郭蕾[1] 屈凌波[1] 赵玉芬[1] 

机构地区：[1]郑州大学化学生物学重点实验室郑州大学化学系,河南郑州450052

出　　处：《波谱学杂志》2003年第2期161-165,共5页Chinese Journal of Magnetic Resonance

基　　金：国家自然科学基金资助项目 (39870 4 15); 2 0 0 1河南省省拨院士基金资助项目

摘　　要：在冰盐浴条件下 ,将DEPH和CCl4混合液滴加到由苯酚、三乙胺、二氧六环组成的混合液中或由水杨酸乙酯 ,三乙胺、二氧六环组成的混合液中 .分别用二乙基亚磷酸酯(DEPH)对苯酚和水杨酸乙酯进行磷酰化 .经电喷雾质谱 (ESI MS)及核磁共振检测 ,目标产物存在 ,其分别为磷酸苯基二乙基酯和o (邻乙氧甲酰 (基 )苯基 )磷酸二乙酯 .The Atheron-Todd reaction has been used extensively for the synthesis of phosphates and phosphoroamidates. In this study, phenol and eyhyl-salicylate were phosphorylated by a modified Atheron-Todd procedure through dropping DEPH and tetrachloromethane into a solution mixture of phenol, triethylamine and dioxane and a solution mixture of ethyl-salicylate, triethylamine and dioxane respectively. Two diethyl substituted phenyl phosphates were obtained with good yields, their structures were elucidated by NMR and ESI-MS/MS.

关 键 词：磷酸苯基二乙基酯 合成 NMR 磷酰化 电喷雾质谱 ESI-MS 核磁共振 苯酚 水杨酸乙酯 o—(邻乙氧甲酰(基)苯基)磷酸二乙酯 

分 类 号：O627.51[理学—有机化学]