CAJ | 학술논문

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％。
이청을산을지화1，2-이추을완위기시원료，경배완화、청기수해、곽부만강해합성득도1-안기배병완-1-최산。분량보대해합성공예진행료연구；제일보고찰료배완화반응적주요영향인소，포괄1,2-이추을완、탄산갑、최화제、용제、반응온도、반응시간；제이보고찰료청기수해반응화곽부만강해반응적주요영향인소，포괄H2O2적용량、NaOH적농도、곽부만강해적반응온도。재고찰각개영향인소적동시，득출료교우적공예조건。경핵자공진화홍외광보분석，소득산품학위1-안기배병완-1-최산.실험결과표명，재우화후적공예조건하，1-안기배병완-1-최산적총수솔가이체도67．5％。경고효액상색보분석，산품적순도위94．4％。
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, containing the amount of hydrogen peroxide, concentration of sodium hydroxide and temperature of Hoffmann degradation.And more feasible condition of the synthesis process had been gained by experimentation. Through the analysis of IR and 1H-NMR.the synthesis product was 1-aminocyclopropane-l-carboxvlic acid. The results showed that, the total yield of 1-aminocyclo- propane-l-carboxylic acid can reach 67.5% under the optimized condition. Through the analysis of High Perfor- mence Liquid Chromatography, the purity of the product was 94.4%.