第 38 卷第 1 期Vol. 38 No. 1
2008 年 2 月Feb 2008

所属栏目:有机合成原料

重氮乙酸乙酯的合成与含量分析
王红利1,2,刘改玲1,2,李争宁1,2,陈惠麟3 (1. 大连大学 环境与化工学院,辽宁 大连 116622;2. 辽宁省生物有机化学重点实验室,辽宁 大连 116622;3. 中国科学院 大连化学物理研究所,辽宁 大连116023)
摘 要:对亚硝酸钠与甘氨酸乙酯盐酸盐合成重氮乙酸乙酯的过程进行了改进,在滴加亚硝酸钠前给体系中加入适量强酸可以促进反应平稳进行,收率达95.8%,建立了用紫外光谱法测定溶液中重氮乙酸乙酯的方法。该合成方法经工业实验,适于大规模生产。
关键词:重氮乙酸乙酯;合成;分析;重氮化
中图分类号:TQ225.24+1  文献标识码:A  文章编号:1009-9212(2008)01- 0040-04
The Synthesis and Analysis of Ethyl Diazoacetate
WANG Hong-li1,2,LIU Gai-ling1,2,LI Zheng-ning1,2,CHEN Hui-lin3 (1. College of Environmental and Chemical Engineering,Dalian University,Dalian 116622,China;2. Liaoning Key Laboratory of Bioorganic Chemistry,Dalian 116622,China;3. Dalian Institute of Chemical Physics,The Chinese Academy of Sciences,Dalian 116023,China)
Abstract:The procedure for the preparation of ethyl diazoacetate via the reaction of sodium nitrate with ethyl glycinate hydrochloride was modified. Strong acid was added to the reaction media prior to the addition of sodium nitrate to promote the reaction proceeding steadily, and the yield reached 95.8% under the optimal conditions. A method for determining the concentration of ethyl diazoacetate by UV spectroscopy was developed. The procedure was applicable to large scale preparation.
Key words:ethyl diazoacetate;synthesis;analysis;diazotization
作者简介:王红利(1984-),男,陕西商洛人,研究方向:精细化学品的合成。(E-mail: hlwang1984@yahoo.com.cn)
联 系 人:李争宁,教授,从事精细化学品的合成与开发。(E-mail: znli@dl.cn)
收稿日期:2007-11-18