第 46 卷第 1 期Vol. 46 No. 1
2016 年 2 月Feb 2016

所属栏目:医药及中间体

2-N,N-双(2-羟基乙氧基乙基)氨基-4-乙酰氨基苯甲醚的合成工艺研究
朱金林1,沈大冬1,王 鼐2,杨红伟2,程广斌2* (1. 浙江医药股份有限公司,浙江 新昌 312500;2. 南京理工大学 化工学院,江苏 南京 210094)
摘 要:以2-氨基-4-乙酰氨基苯甲醚与2-(2-氯乙氧基)乙醇为原料合成了未见报道的化合物2-N,N-双(2-羟基乙氧基乙基)氨基-4-乙酰氨基苯甲醚。考察了不同的反应条件,如缚酸剂种类和用量、投料比、反应温度和催化剂等因素对产品收率和纯度的影响。优化条件下,产物收率79.9%,纯度98.7%。
关键词:2-氨基-4-乙酰氨基苯甲醚;2-(2-氯乙氧基)乙醇;2-N,N-双(2-羟基乙氧基乙基)氨基-4-乙酰氨基苯甲醚
中图分类号:Q625.1  文献标识码:A  文章编号:1009-9212(2016)01-0034-05
Synthesis and Technique Optimization of 2-(N,N-bis((2-hydroxyethoxy)ethyl)amino)-4-acetamino)anisole
ZHU Jin-lin1, SHEN Da-dong1, WANG Nai2, YANG Hong-wei2, CHENG Guang-bin2* (1. Zhejiang Medicine Co., Ltd., Xinchang 312500, China; 2. School of Chemical Engineering, Nanjing University of Science and Techonology, Nanjing 210094, China)
Abstract:New compound of 2-(N,N-bis((2-hydroxyethoxy)ethyl)amino)-4-acetamino)anisole was synthesized by the reaction of 2-amino-4-acetamino anisole with 2-(2-chloroethoxy)ethanol. The effects of reaction conditions on the yield and purity were investigated, including the kinds of acid binding agent, the amount of acid binding agent, feed ratio, reaction temperature and catalyst. The results showed that yield of the product would increase with the weakening alkaline acid binding agent. And the yield rate of the product after the first increases and then decreases with the addition of amount of acid-binding agent, amount of 2-(2-chloroethoxy)ethanol and the reaction time.
Key words:2-amino-4-acetamino anisole; 2-(2-chloroethoxy)ethanol; 2-(N,N-bis((2-hydroxyethoxy)ethyl)amino)-4-acetamino)anisole
基金项目:国家自然科学基金项目(21376121)
作者简介:朱金林(1975-),男,江苏泰兴人,高级工程师,硕士,研究方向:仪器分析与质量控制(E-mail:zjl@xcpharma.com)。
联 系 人:程广斌,教授,研究方向:有机合成化学研究(E-mail:gcheng@mail.njust.edu.cn)。
收稿日期:2016-01-28