摘要
[目的]考察N-苄基甘氨酸乙酯的合成工艺条件。[方法]以甘氨酸乙酯盐酸盐为原料,与氯化苄经N-烷基化反应合成N-苄基甘氨酸乙酯,研究反应温度、投料比、缚酸剂、溶剂等因素对试验结果的影响。[结果]优化工艺条件为:40℃反应4h,n(氯化苄):n(甘氨酸乙酯盐酸盐)为1.1∶1,三乙胺为缚酸剂,乙醇为溶剂,收率80.3%(以甘氨酸乙酯盐酸盐计),纯度98.0%(GC)以上。[结论]改进后的合成工艺操作简便,收率与纯度均较高,生产成本较低,为大规模生产N-苄基甘氨酸乙酯提供理论依据。
[Objective]To investigate the synthesis process conditions of N-benzylglycine ethyl ester. [Method]N-Benzylglycine ethyl ester was synthesized from glycine ethyl ester hydrochloride and benzyl chloride via N-alkylation reaction. The optimum conditions for synthesis were studied by investigating effects of temperature,molar ratio of raw materials,acid-binding agents,solvent etc. on experiment results. [Result]The improved synthesis process conditions for reaction were as follows:reaction temperature 40 ℃,reaction time 4h,the molar ratio of benzyl chloride and glycine ethyl ester hydrochloride was 1. 1∶1,acid-binding agent triethylamie,solvent ethanol ,the yield was 80. 3% ,the purity was above 98. 0% (GC). [Conclusion]The improved synthetic route was convenient,relative low-cost,yield and purity were better,which provided theoretical basis for large-scale synthesis of N-benzylglycine ethyl ester.
出处
《安徽农业科学》
CAS
北大核心
2010年第14期7694-7695,共2页
Journal of Anhui Agricultural Sciences
基金
江苏省自然科学基金资助项目(BK2009523)
江苏省高校自然科学基金资助项目(09KJB350003)
江苏省高校自然科学基金资助项目(08KJD530004)
徐州市科技计划项目(XM08C059)
徐州医学院肿瘤生物治疗实验室资助项目(C0903)
江苏省高等学校大学生实践创新训练计划项目(2008)
关键词
N-苄基甘氨酸乙酯
农药和医药中间体
合成
N-烷基化
N-benzylglycine ethyl ester
Pesticide and pharmaceutical intermediate
Synthesis
N-alkylation