化工进展

• 精细化工 • 上一篇    下一篇

(S)-2-苄氧基丙醛的合成及结构表征

徐东超1,曲敏杰1,姜殿平2,李成斌2,郭 静1,阮久勇1   

  1. 1大连工业大学纺织与材料工程学院,辽宁 大连 116034;2大连奇凯医药科技有限公司,辽宁 大连 123000
  • 出版日期:2012-06-05 发布日期:2012-06-25

Synthesis and characterization of(S)-2-benzyloxyl propanal

XU Dongchao1,QU Minjie1,JIANG Dianping2,LI Chengbin2,GUO Jing1,RUAN Jiuyong1   

  1. 1School of Textile and Material Engineering,Dalian Polytechnic University,Dalian 116034,Liaoning,China; 2Dalian Qi-Chem Pharmaceutical Technology Company Limited,Dalian 123000,Liaoning,China
  • Online:2012-06-05 Published:2012-06-25

摘要: (S)-2-苄氧基丙醛是有机合成及制药的重要中间体,本文以(S)-乳酸乙酯为原料,经四氢吡咯胺化、氯化苄醚化、红铝还原反应合成了(S)-2-苄氧基丙醛,考察了胺化的反应时间、反应温度和原料的摩尔比对反应收率的影响。结果表明:当胺化反应时间为75 h,最佳的反应温度为25 ℃,四氢吡咯与(S)-乳酸乙酯的摩尔比为1.4∶1时,胺化反应收率为94%,三步总收率为61.8%,采用GC-MS、IR、1H NMR表征确定了产物结构,研究结果为(S)-2-苄氧基丙醛的工业化生产奠定了基础。

关键词: (S)-乳酸乙酯, 胺化反应, (S)-2-苄氧基丙醛, 合成

Abstract: Vanadium redox flow battery is a highly efficient storage energy installs. The electrolyte influence the battery capacity directly. (S)-2 - benzyloxy propanal was synthesized by the amination of pyrrolidine,the etherification of benzyl chlorine and sodium bisaluminiumhydride with ethyl(S)-lactate as raw material. The reaction time ,the reaction temperature and the mole ratio of raw material in the process of amination were investigated. The results showed that the yield of amination reaction was about 94% when amination reaction time was 72 h,the reaction temperature was 25 ℃ and the mole ratio of pyrrolidine to ethyl(S)-lactate was 1.4∶1. The overall yield was about 61.8%. The product structure was characterized and confirmed by GC-MS,IR and 1H NMR. The results provided important theoretical base for the industrial production of(S)-2 - benzyloxy propanal.

Key words: ethyl(S)-lactate, amination reaction, (S)-2-benzyloxyl propanal, synthesis