胡椒酸己二胺的合成

以胡椒碱为起始原料，与KOH反应生成胡椒酸钾盐，经酸化后制得胡椒酸(2)； 2与乙醇经酯化反应制得胡椒酸乙酯(3)； 3与己二胺在金属钠催化下经氨解反应合成了胡椒酸己二胺(4)，其结构经¹H NMR, ¹³C NMR和IR确证。合成4的最佳反应条件为：催化剂用量2 wt%， n(3):n(己二胺)=0.6， m(乙醇):m(3)=2.5，于65～75 ℃反应48 h，收率83.5%。该工艺在微型实验基础上放大十倍，收率大于79%。

Synthesis of Pepper Acid Hexamethylene Diamine

Piperic acid(2) was prepared by reaction of piperine with KOH , and then acidification. Ethyl piperic acid(3) was prepared by reaction of 2 with ethanol.Pepper acid hexanediamine (4) was obtained by ammonolysis of 3 with hexamethylene diamine catalyzed by sodium .The structure was con-firmed by 1 H NMR, 13 C NMR and IR.The optimum reaction conditions for synthesizing 4 were as fol-lowed:The catalyst dosage was 2 wt%, n(3)∶n(hexamethylenediamine ) =0.6, reaction at 65~75℃for 48 h, the yield was 83 .5%.The process was magnified by ten times on the micro experiment , the yield was above 79%.