论文部分内容阅读
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%。
Piperine is used as a starting material to react with KOH to produce a salt of piperonyl peracid and acidified to produce piperonyl acid (2); 2 ethyl ester of piperonyl ethyl acetate (3) is formed through esterification with ethanol; 3 is reacted with hexamethylenediamine Hexamethylenediamine hexahydrate (4) was synthesized by aminolysis catalyzed by sodium metal, and its structure was confirmed by ~ 1H NMR, ~ (13) C NMR and IR. The optimal reaction conditions for the synthesis of 4 were as follows: the amount of catalyst was 2 wt%, n (3): n (hexamethylenediamine) = 0.6, m (ethanol) Yield 83.5%. The process on the basis of micro-experiments enlarged ten times, yield greater than 79%.