| 3-(N,N-二甲氧基乙基)氨基乙酰苯胺合成工艺优化研究 |
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| 引用本文： | 向海艳,宁静恒.3-(N,N-二甲氧基乙基)氨基乙酰苯胺合成工艺优化研究[J].精细化工中间体,2010,40(3):44-46. |
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| 作者姓名： | 向海艳 宁静恒 |
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| 作者单位： | 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 |
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| 基金项目： | 广东省教育部产学研结合项目 |
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| 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。
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| 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 |
Optimization of Synthetic Technique for 3-(N,N-Dimethoxyethyl)amino Acetanilide |
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| XIANG Hai-yan,NING Jing-heng.Optimization of Synthetic Technique for 3-(N,N-Dimethoxyethyl)amino Acetanilide[J].Fine Chemical Intermediates,2010,40(3):44-46. |
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| Authors: | XIANG Hai-yan NING Jing-heng |
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| Affiliation: | 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) |
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| 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. |
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| Keywords: | 3-（N N-dimethoxyethyl）amino acetanilide 2-chloroethyl methyl ether 3-amino acetanilide methyl ether |
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