稳定同位素氘标记盐酸曲托喹酚的制备  

Preparation of Stable Isotope Deuterium Labeled Tretoquinol Hydrochloride

作　　者：秦爽 韩世磊 邵文哲 徐银 石静飞 佟庆龙 张磊 QIN Shuang;HAN Shi-lei;SHAO Wen-zhe;XU Yin;SHI Jing-fei;TONG Qing-long;ZHANG Lei(Alta Scientific Co.,Ltd.,Tianjin 300457,China;Alta Institute of Reference Materials Co.,Ltd.,Tianjin 300457,China)

机构地区：[1]天津阿尔塔科技有限公司,天津300457 [2]阿尔塔标准物质研究院,天津300457

出　　处：《化学试剂》2022年第4期599-603,共5页Chemical Reagents

基　　金：国家重点研发计划项目(2019YFC1604804)。

摘　　要：以2-(3,4,5-三甲氧基苯基)乙酸为起始原料,经过脱甲基、酰胺化、甲基化、比希勒-纳皮拉尔斯基(Bischler-Napieralski)环化反应、还原、脱保护基等关键反应步骤,得到稳定同位素氘标记的盐酸曲托喹酚。该合成方法原料廉价易得、简单成熟,目标产物氘同位素丰度较高。该产物经核磁共振氢谱(^(1)HNMR)和高分辨质谱(HR-MS)表征确认,氘同位素丰度为99.9 atom%D,适合作为同位素标记质谱内标试剂用于曲托喹酚的定性定量分析。A novel deuterium labelled tretoquinol hydrochloride was synthesized from 2-(3,4,5-trimethoxyphenyl) acetic acid via the steps of demethylation,amidation,alkylation,Bischler-Napieralski cyclization reaction,reductive,and deprotection.The synthetic route has the advantages of cheap,accessible starting materials and high isotope abundance.The deuterium-labelled product was confirmed by nuclear magnetic resonance(^(1)HNMR) and high-resolution mass spectrometry(HR-MS) characterization with 99.9 atom% D deuterium isotope abundance,which can be used as stable isotope-labeled MS internal standards for qualitative and quantitative analysis.

关 键 词：稳定同位素标记 氘标记盐酸曲托喹酚 质谱内标试剂 同位素丰度 

分 类 号：O628.1[理学—有机化学]