第 40 卷第 3 期 |  | Vol. 40 No. 3 | 2010 年 6 月 | Jun 2010 |
|
所屬欄目:染料、顏料及涂料
3-(N,N-二甲氧基乙基)氨基乙酰苯胺合成工藝優(yōu)化研究 |
向海艷1,寧靜恒2
(1. 南方醫科大學(xué) 藥學(xué)院,廣東 廣州,510515;2. 長(cháng)沙理工大學(xué) 化學(xué)與環(huán)境工程學(xué)院,湖南 長(cháng)沙,410076) |
摘 要:優(yōu)化了用2-氯乙基甲醚和間氨基乙酰苯胺合成3-(N,N-二甲氧基乙基)氨基乙酰苯胺的工藝條件。首次采用N,N-二甲基甲酰胺催化合成原料2-氯乙基甲醚,明顯縮短了反應時(shí)間并獲得較高收率。在3-(N,N-二甲氧基乙基)氨基乙酰苯胺的合成中,使用普通縛酸劑純堿,采用分批加入原料、補充縛酸劑和分階段升溫的方式,有效控制了原料的水解問(wèn)題,產(chǎn)品收率達98%。筆者研究成果已應用于工業(yè)化生產(chǎn)。 |
關(guān)鍵詞:3-(N,N-二甲氧基乙基)氨基乙酰苯胺;2-氯乙基甲醚;間氨基乙酰苯胺 |
中圖分類(lèi)號:TQ246 文獻標識碼:A 文章編號:1009-9212(2010)03-0044-03 |
|
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 |
|
基金項目:廣東省教育部產(chǎn)學(xué)研結合項目(2009B090300216)。
|
作者簡(jiǎn)介:向海艷(1974-),女,湖南龍山人,講師,博士,主要從事精細化學(xué)品方面的研究。(E-mail:xhy330@126.com )
|
收稿日期:2010-05-29
|
|