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

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.