1-氨基环丙烷-1-羧酸的合成工艺研究与优化

以氰乙酸乙酯和1,2-二溴乙烷为起始原料,经环烷化、氰基水解、霍夫曼降解合成得到1-氨基环丙烷-1-羧酸。分两步对该合成工艺进行了研究:第一步考察了环烷化反应的主要影响因素,包括1,2-二溴乙烷、碳酸钾、催化剂、溶剂、反应温度、反应时间;第二步考察了氰基水解反应和霍夫曼降解反应的主要影响因素,包括H2O2的用量、NaOH的浓度、霍夫曼降解的反应温度。在考察各个影响因素的同时,得出了较优的工艺条件。经核磁共振和红外光谱分析,所得产品确为1-氨基环丙烷-1-羧酸。实验结果表明,在优化后的工艺条件下,1-氨基环丙烷-1-羧酸的总收率可以达到67.5%。经高效液相色谱分析,产品的纯度为94.4%。

Study on the Synthesis of 1-Aminocyclopropane-1-carboxylic Acid

1-Aminocyclopropane-1-carboxylic acid was synthesized by cycloalkylation,hydrolysis of cyano group,Hoffmann degradation from ethyl cyanoacetate and 1,2-dibromethane in this article.There were two steps of the synthesis process in this research.First,the major factors of cycloalkylation reaction were studied,containing 1,2-dibromethane,potassium carbonate,catalyst,solvent,reaction temperature and reaction time.Second,the major factors of hydrolysis of cyano group and Hoffmann degradation were studied,contain...