第 43 卷第 6 期 | | Vol. 43 No. 6 | 2013 年 12 月 | Dec 2013 |
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所属栏目:医药及中间体
对氯肉桂酸甲酯的一锅法绿色合成 |
李 贺,田 丹,曾庆友*
(华侨大学 化工学院,福建 厦门 361021) |
摘 要:以对氯苯甲醛、丙二酸二乙酯为主要原料,甘氨酸为催化剂,无水甲醇为溶剂,经水解、酸化和Knoevenagel缩合等反应一锅法合成了对氯肉桂酸甲酯。考察了反应物配比、催化剂用量、反应时间及溶剂用量等因素对产物收率的影响。优化反应条件为:n(对氯苯甲醛)∶n(丙二酸二乙酯)∶ n(甘氨酸)=1.0∶1.4∶0.35,反应时间8 h时,收率87.3%,纯度达99.2%。合成方法操作简单,环境污染少,有工业应用前景。 |
关键词:对氯肉桂酸甲酯;甘氨酸;Knoevenagel缩合;一锅法 |
中图分类号:TQ251.1 文献标识码:A 文章编号:1009-9212(2013)06-0022-03 |
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One-pot Synthesis of Methyl p-Chlorocinnamate |
LI He,TIAN Dan,ZENG Qing-you*
(College of Chemical Engineering,Huaqiao University,
Xiamen 361021,China) |
Abstract:Methyl p-chlorocinnamate was synthesized from p-chlorobenzaldehyde and diethyl malonate under catalysis of glycine in methanol. The effects of molar ratio of reactants,dosage of catalyst,reaction time and dosage of solvent on the reaction were investigated. The optimal reaction conditions include n(diethyl malomate)∶n(p-chlorobenzaldehyde)=1.4∶1,n(glycine)∶n(p-chlorobenzaldehyde)= 0.35∶1,and reaction time 8 h. The yield of methyl p-chlorocinnamate was up to 87.3% with 99.2% purity. This method is simple,safe,environmental friendly and suitable for industrial
production. |
Key words:methyl p-chlorocinnamate;glycine;Knoevenagel
condensation;one-pot synthesis |
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基金项目:国家自然科学基金培育计划专项项目(11J0228)。
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作者简介:李 贺(1987-),男,安徽阜阳人,硕士研究生,主要从事精细化工中间体合成。(E-mail:lihe20052005@126.com)
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联 系 人:曾庆友,副教授,主要从事有机合成及高分子载体合成。(E-mail:tonyzeng@hqu.edu.cn)
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收稿日期:2013-11-08
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