15-二氘脱水穿心莲内酯的合成和氢-氘交换速率考察  

The Synthesis of 15-Dideuteriumdehydroandrographolide and Test of The Hydrogen-deuterium Exchange Rate

作　　者：霍志鹏 刘迪 邱峰[1] HUO Zhi-peng;LIU Di;QIU Feng(State Key Laboratory of Component-based Chinese Medicine, School of Chinese Materia Medica, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China)

机构地区：[1]天津中医药大学中药学院组分中药国家重点实验室,天津301617

出　　处：《合成化学》2021年第8期710-714,共5页Chinese Journal of Synthetic Chemistry

基　　金：国家自然科学基金资助项目(81873079)。

摘　　要：以脱水穿心莲内酯为原料,氧化氘作为氘源,四氢呋喃为助溶剂,三乙胺催化反应,分离纯化得到反应产物,其结构经^(1)H NMR、^(13)C NMR和HR-MS(ESI-TOF)确证,并考察了产物在不同pH值的氢氘交换速率。结果显示,产物表征鉴定为15-二氘脱水穿心莲内酯,15位H-D交换速率在pH分别为6,7和8时较慢,随pH值升高加快。Dehydroandrographolide was used as raw material,deuterium oxide as deuterium source,tetrahydrofuran as co-solvent,and triethylamine as catalyst.The product was obtained by separation and purification,and their structures were confirmed by ^(1)H NMR,^(13)C NMR and HR-MS(ESI-TOF).The reaction product was identified as 15-dideuteriumdehydroandrographolide.The 15-H-D exchange rate of C-15 position was slow in pH 6,7,8 buffer solutions,and elevated as pH value arise.

关 键 词：15-二氘脱水穿心莲内酯 氘代合成 碱催化 氢-氘交换速率 PH 

分 类 号：O621.3[理学—有机化学]