[an error occurred while processing this directive]
化学工业与工程
 首页 |  在线投稿 |  期刊介绍 |  编 委 会 |  投稿指南 |  期刊订阅 |  下载中心 |  出版伦理 |  联系我们 |  English
化学工业与工程 2014, Vol. 31 Issue (4) :22-25    DOI: doi: 10.13353/j.issn.1004.9533.2014.04.005
化学反应与工艺 最新目录 | 下期目录 | 过刊浏览 | 高级检索 << | >>
Duff反应法合成5-壬基水杨醛
赵莹茜,王李和,李效军
(河北工业大学化工学院,天津 300130)
Synthesis of 5-Nonylsalicyaldehyde by Duff Reaction
ZHAO  Ying-Qian, WANG  Li-He, LI  Xiao-Jun
(School of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130, China)

摘要
参考文献
相关文章
Download: PDF (1338KB)   HTML ()   Export: BibTeX or EndNote (RIS)      Supporting Info
摘要 5-壬基水杨醛是合成5-壬基水杨醛肟的重要中间体,5-壬基水杨醛肟作为铜萃取剂在工业上有很多应用。以4-壬基酚、六次甲基四胺为原料,醋酸为溶剂,经Duff反应合成了5-壬基水杨醛。相对其他合成5-壬基水杨醛的方法,采用Duff反应来合成具有操作简便、反应周期较短、产物单一且容易进行提纯等优点。通过对原料的物质的量之比、反应时间、反应温度等因素对目标产物收率的影响,确定了合成5-壬基水杨醛适宜的反应条件:n(4-壬基酚)∶n(六次甲基四胺)=1∶2,反应温度为90 ℃,醋酸为溶剂,反应6 h。在上述条件下,以4-壬基酚计,目标产物的收率为98.7%,液相色谱纯度为92.0%,产物经1H-NMR表征,其结构目标产物一致。
Service
把本文推荐给朋友
加入我的书架
加入引用管理器
Email Alert
RSS
作者相关文章
赵莹茜
王李和
李效军
关键词5-壬基水杨醛;   4-壬基酚;   甲酰化;   六次甲基四胺     
Abstract: 5-Nonylsalicylaldehyde was the important intermediates in the synthesis of 5-nonylsalicylaldoxime, which as copper extraction agent had many applications in industry. In this paper, 5-nonylsalicyaldehyde was synthesized from 4-nonylphenol, hexamethylenetetramine in acetic acid via Duff reaction. Compared to the other synthesis methods, the synthesis method of 5-nonylsalicyaddehyde used Duff reaction has much advantages, such as simple operation, short reaction period, single product and easy to be purified. The effects of reactant mole ratio, reaction temperature, reaction time on the reaction yield were studied. The optimum reaction conditions were as follows: n(4-nonylphenol):n(hexamethylenetetramine)=1:2 and the reaction mixture was dissolved in acetic acid and stirred at 90 ℃ for about 6 h. Under these conditions, the yield of 5-nonylsalicyaldehyde was 98.7% based on 4-nonylphenol with a purity of 92.0% (analyzed by HPLC). Structure of the product was elucidated by 1H-NMR analysis.
Keywords5-nonylsalicylaldehyde;   4-nonylphenol;   formylation;   hexamethylenetetramine     
Received 2014-04-04;
Corresponding Authors: 李效军,电话:(022)26582469。      Email: lixiaojun@hebut.edu.cn
About author: 赵莹茜(1989-),女,硕士研究生,应用化学专业,主要研究精细化学品的合成。
引用本文:   
赵莹茜, 王李和, 李效军.Duff反应法合成5-壬基水杨醛[J].  化学工业与工程, 2014,31(4): 22-25
ZHAO Ying-Qian, WANG Li-He, LI Xiao-Jun.Synthesis of 5-Nonylsalicyaldehyde by Duff Reaction[J].  Chemcial Industry and Engineering, 2014,31(4): 22-25
Copyright 2010 by 化学工业与工程