稳定性同位素氘标记对羟基苯甲酸正丁酯的合成与表征  

Synthesis and Characterization of Stable Isotope Deuterium Labelled Butyl 4-Hydroxybenzoate

作　　者：王伟[1] 王雪婷[1] 杜晓宁[1] 

机构地区：[1]上海化工研究院上海稳定性同位素工程技术研究中心,上海200062

出　　处：《化学试剂》2017年第7期755-758,共4页Chemical Reagents

基　　金：科技部"十二五"重点支撑计划项目(2015BAK-45B-20)

摘　　要：以对羟基苯甲酸-环-D4为同位素原料,酸性条件下与正丁醇反应得到对羟基苯甲酸正丁酯-环-D4。考察了酸性催化剂种类对产物同位素丰度的影响,筛选出最佳酸性催化剂对甲苯磺酸。通过单因素实验得到优化后的工艺参数,n(正丁醇)∶n(对羟基苯甲酸-环-D_4)=5∶1,m(对甲苯磺酸)∶m(对羟基苯甲酸-环-D_4)=0.05∶1,反应温度为95℃,反应时间为4.5 h。产物经GC-MS、~1HNMR和FT-IR进行分析,化学纯度>99.0%,同位素丰度>97 atom%D。A new procedure for the synthesis of the deuterium labelled butyl 4-hydroxybenzoate has been developed.The effects of acid catalysts types on isotope abundance of butyl 4-hydroxybenzoate-ring-D4 were investigated,and p-toluene sulfonic acid was chosen as the catalyst.The optimal reaction conditions were obtained as follows：The molar ratio of butyl alcohol to 4-hydroxybenzoic acid-ring-D4 was 5∶1,the mass ratio of p-toluene sulfonic acid to 4-hydroxybenzoic acid-ring-D4 was 0.05∶1,the temperature was 95 ℃,the reaction time was 4.5 h.The chemical purity was above 99.0%,and the isotopic abundance was above 97 atom%D.The product butyl 4-hydroxybenzoate-ring-D4 was carried out by GC-MS,-1HNMR and FT-IR.

关 键 词：同位素内标试剂 对羟基苯甲酸正丁酯 尼泊金丁酯 稳定同位素标记 氘标记试剂 

分 类 号：O628.2[理学—有机化学]