六氟异丙醇促进的二甲基吡啶胺合成工艺研究  

Studies on the Synthesis Process of 2,2'-Dipicolylamine Promoted by 1,1,1,3,3,3-Hexafluoro-2-propanol

作　　者：肖林霞 亓亮 凌柏 Xiao Linxia;Qi Liang;Ling Bai(Department of Pharmacy,Jiangsu Vocational College of Medicine,Yancheng,Jiangsu 224005,China;Departement of Hospital Pharmacy,Yancheng No.1 People's Hospital,Yancheng,Jiangsu 224000,China)

机构地区：[1]江苏医药职业学院药学系,江苏盐城224005 [2]盐城市第一人民医院药房,江苏盐城224000

出　　处：《化学世界》2023年第2期116-118,共3页Chemical World

基　　金：江苏省高等学校自然科学研究面上(No.19KJB350010);博士启动经费(No.20186104)资助项目。

摘　　要：以2-氨甲基吡啶(1)和2-吡啶甲醛(2)为原料、NaBH4为还原试剂,在六氟异丙醇(HFIP)中制备二甲基吡啶胺(3),对反应溶剂、还原试剂和溶剂循环次数等工艺参数进行了优化,并进行了百克级放大。结果表明,HFIP作为高极性溶剂,可以有效促进二甲基吡啶胺的合成,在最优条件下(HFIP,r.t.~reflux,体积分数为10%甲醇,NaBH_(4)),产率为80.46%,HFIP可以进行多次循环使用。2,2'-Dipicolylamine(3)was prepared usingg2-aminomethylpyridine(1)and 2-pyridinecarboxaldehyde(2)as raw materials and NaBH,as reductant in 1,1,1,3,3,3-hexafluoro-2-propanol(HFIP).The process parameters such as solvent,reductant and solvent cycle number were optimized.The process has been scaled up at hundred grams level and the results showed that HFIP,as a highly polar solvent,can effectively promote the synthesis of 2,2'-dipicolylamine.The yield is 80.46%under optimal conditions(HFIP,r.t.~reflux,volume fraction 1o%methanol,NaBH_(4)).Moreover,HFIP can be recycled many times.

关 键 词：六氟异丙醇 二甲基吡啶胺 百克级放大 循环使用 

分 类 号：O625.631[理学—有机化学]