胡椒酸己二胺的合成

Synthesis of Pepper Acid Hexamethylene Diamine

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,^(13)C 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%。

Piperic acid（2） was prepared by reaction of piperine with KOH, and then acidification. Ethyl piperie 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 1H 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%.