应用化学 ›› 2010, Vol. 27 ›› Issue (05): 618-620.DOI: 10.3724/SP.J.1095.2010.90527

• 研究简报 • 上一篇    

超声波辐射下异阿魏酸对氯苯酚酯的一步合成

程青芳1,2*,许兴友1,2,王启发1,林俏1,刘望军1,杨绪杰2   

  1. (1.淮海工学院化学工程系 连云港 222005;2.南京理工大学材料化学实验室 南京 210094)
  • 收稿日期:2009-08-10 修回日期:2009-09-14 出版日期:2010-05-10 发布日期:2010-05-10
  • 通讯作者: 程青芳,女,副教授; E-mail:cheng_qingfang@yahoo.com.cn; 研究方向:药物及中间体的合成
  • 基金资助:
    江苏省海洋资源开发研究院科技开放基金(JSIMR09B03)和连云港市科技攻关项目基金(CG0713)资助项目

One-step Synthesis of 4-Chlorophenyl Isoferulate under Ultrasonic Irradiation

CHENG Qing-Fang1,2*, XU Xing-You1,2, WANG Qi-Fa1, LIN Qiao1, LIU Wang-Jun1, YANG Xu-Jie2   

  1. (1.Deparment of Chemical Technology,Huaihai Institute of Technology,Lianyungang 222005;
    2.Materials Chemistry Laboratory,Nanjing University of Science and Technology,Nanjing 210094)
  • Received:2009-08-10 Revised:2009-09-14 Published:2010-05-10 Online:2010-05-10

摘要:

室温超声辐射下,4-二甲氨基吡啶(DMAP)作催化剂,二环己基碳二亚胺(DCC)作脱水剂,不需保护异阿魏酸分子中的羟基,异阿魏酸和对氯苯酚的一步反应直接合成了异阿魏酸对氯苯酚酯。 在n(异阿魏酸)∶n(对氯苯酚)∶n(DCC)∶n(DMAP)=1∶1.2∶1.2∶0.1混合时,室温超声反应2.5 h,得产率76.2%。 目标化合物的结构经元素分析、1H NMR和IR测试技术得到确证。 缩短了反应时间,提高了产率。

关键词: 异阿魏酸对氯苯酚酯, 二环己基碳二亚胺, 4-二甲氨基吡啶, 超声辐射

Abstract:

4-Chlorophenyl isoferulate was synthesized in onestep from isoferulic acid and 4-chlorophenol without the protection of the hydroxyl of isoferulic acid in the presence of 4-dimethylpyridine(DMAP) as catalyst and dicyclohexylcarbodiimide(DCC) as dehydrating agent under ultrasonic irradiation at room temperature. When reactants were mixed in a n(isoferulic acid)∶n(4-chlorophenol)∶n(DCC)∶n(DMAP)=1∶1.2∶1.2∶0.1, and exposed to ultrasonic irradiation for 2.5 h, the yield was 76.2%. The structure of the product was confirmed by elemental analysis, 1H NMR and IR. This method avoids the long reaction time and increases the yield compared with traditional synthetic method.

Key words: 4-chlorophenyl isoferulate, dicyclohexylcarbodiimide, 4-dimethylpyridine, ultrasonic irradiation

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