第 40 卷第 3 期 | | Vol. 40 No. 3 | 2010 年 6 月 | Jun 2010 |
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所属栏目:染料、颜料及涂料
3-(N,N-二甲氧基乙基)氨基乙酰苯胺合成工艺优化研究 |
向海艳1,宁静恒2
(1. 南方医科大学 药学院,广东 广州,510515;2. 长沙理工大学 化学与环境工程学院,湖南 长沙,410076) |
摘 要:优化了用2-氯乙基甲醚和间氨基乙酰苯胺合成3-(N,N-二甲氧基乙基)氨基乙酰苯胺的工艺条件。首次采用N,N-二甲基甲酰胺催化合成原料2-氯乙基甲醚,明显缩短了反应时间并获得较高收率。在3-(N,N-二甲氧基乙基)氨基乙酰苯胺的合成中,使用普通缚酸剂纯碱,采用分批加入原料、补充缚酸剂和分阶段升温的方式,有效控制了原料的水解问题,产品收率达98%。笔者研究成果已应用于工业化生产。 |
关键词:3-(N,N-二甲氧基乙基)氨基乙酰苯胺;2-氯乙基甲醚;间氨基乙酰苯胺 |
中图分类号:TQ246 文献标识码:A 文章编号:1009-9212(2010)03-0044-03 |
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Optimization of Synthetic Technique for 3-(N,N-Dimethoxyethyl)amino Acetanilide |
XIANG Hai-yan1,NING Jing-heng2
(1. School of Pharmaceutical Sciences,Southern Medical University,Guangzhou 510515,China;2. School of Chemistry and Engineering,Changsha University of Science and Technology,Changsha 410004,China) |
Abstract:The synthetic technique for the title compound was optimized via 2-chloroethyl methyl ether and 3-amino acetanilide. DMF was used as the catalyst for the first time for the synthesis of 2-chloroethyl methyl ether,which showed shorter reaction time and afforded higher yield. In this process the acid-binding agent sodium carbonate and the reagents were added in batches and the temperature was increased in 2 steps,which efficiently prevented the starting material from hydrolysis and gave the product in 98% yield. This technique has been commercialized. |
Key words:3-(N,N-dimethoxyethyl)amino acetanilide;2-chloroethyl methyl ether;3-amino acetanilide. methyl ether |
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基金项目:广东省教育部产学研结合项目(2009B090300216)。
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作者简介:向海艳(1974-),女,湖南龙山人,讲师,博士,主要从事精细化学品方面的研究。(E-mail:xhy330@126.com )
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收稿日期:2010-05-29
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