甲基化汉防己乙素制备汉防己甲素的研究和应用  

Preparation of tetrandrine by methylation of fangchinoline and its application

作　　者：丁世磊 吴柳润 梁其钦 郝二伟[2] 邓家刚[2] DING Shilei;WU Liurun;LIANG Qiqin;HAO Erwei;DENG Jiagang(College of Pharmacy,Guangxi University of Chinese Medicine,Nanning 530200,China;Collaborative Innovation Center for Functional Component Research of Crop Waste in Guangxi,Guangxi University of Chinese Medicine,Nanning 530200,China)

机构地区：[1]广西中医药大学药学院,南宁530200 [2]广西中医药大学广西农作物废弃物功能成分研究协同创新中心,南宁530200

出　　处：《药学前沿》2025年第4期560-566,共7页China Pharmacist

基　　金：广西自然科学基金项目(2024GXNSFBA010168);广西中医药大学引进博士科研启动基金项目(2019BS005);农作物废弃物功能成分研究协同创新中心资助课题(CICAR2023-P1);中医药生物新材料关键技术研究与智能装备开发学科交叉创新团队(GZKJ2303)。

摘　　要：目的探寻绿色环保的甲基化汉防己乙素制备汉防己甲素方法,实现浸膏中汉防己乙素向汉防己甲素的转化。方法采用“一锅法”制备汉防己甲素,以HPLC法检测分析产率,通过单因素试验对催化剂、溶剂、反应时间、反应温度、催化剂用量等因素进行探究,筛选出最佳合成工艺。结果在汉防己乙素0.3 g、碳酸二甲酯100μL、N,N-二甲基甲酰胺10 mL、离子液体1-丁基-3-甲基咪唑溴盐([BMIm]Br)1.0 g、反应温度140℃、反应时间2 h、汉防己乙素与碳酸二甲酯摩尔比为1∶2.5的条件下,汉防己乙素几乎完全转化,汉防己甲素产率为62.93%。在该条件下,可以实现浸膏中汉防己乙素向汉防己甲素的转化。结论试验探究得到了绿色环保的汉防己甲素合成新方法,成功将汉防己乙素转换成汉防己甲素。Objective To seek a green and environmentally friendly method to prepare tetrandrine from methylated fangchinoline and realize the transformation of fangchinoline to tetrandrine in the extract.Methods The"one-pot method"was used to prepare tetrandrine.The catalyst,solvent,reaction time,reaction temperature,solid-liquid ratio and other factors were explored by single factor test,and the tetrandrine content was detected by HPLC to screen out the best synthesis process.Results Under the conditions of 0.3 g of frangchinoline,100μL of dimethyl carbonate,10 mL of N,N-dimethylformamide,1.0 g of ionic liquid[BMIm]Br,reaction temperature of 140°C,reaction time of 2 h,and the molar ratio of fangchinoline to dimethyl carbonate of 1∶2.5,the transformation of fangchinoline was almost complete.The target product of tetrandrine was successfully synthesized with a yield of 62.93%.Under these conditions,it was possible to achieve the transformation of fangchinoline to tetrandrine in the extract.Conclusion The experiment has explored a new green synthesis method,which can successfully convert the frangchinoline to tetrandrine.

关 键 词：甲基化 汉防己甲素 离子液体 一锅法 

分 类 号：F416.7[经济管理—产业经济]