摘要
以对乙酰氨基苯磺酰氯(ASC)和乙胺为原料,经胺化反应生成N-(4-乙酰氨基苯磺酰)-乙胺,然后在碱性条件下水解得到N-(4-氨基苯磺酰)-乙胺.实验对胺化条件进行了优化,用HPLC、GC对产物进行了纯度分析,并经FTIR、GC-MS、1 H-NMR对产物进行了结构表征.结果表明,在nASC∶n乙胺=1.1∶1、反应温度为25℃、反应时间为30min时,胺化产率可达74.4%;在95℃下回流3h左右,水解产率为86.7%;纯度分别为96.52%(GC),98.80%(HPLC).该合成方法具有操作简单、收率高、纯度好等优点.
The main raw materials-p-acetamidobenzene sulfonyl chloride and ethylamine,are under amination reaction to produce N-（4-acetamidobenzene sulfonyl）ethylamine,then,the N-（4-aminobenzene sulfonyl）-ethylamine under condition of alkaline hydrolysis.The conditions of amination reaction was optimized in the lab,the products are under purity analysis with HPLC and GC,and are structural characterized through FTIR,GC-MS 1,H-NMR.The result shows that under the conditions of nASC∶nEthylamine=1.1∶1,reaction temperature 25℃,and the reaction time 30 min,the productive rate of amination can reach 74.4%;the backflow at 95℃is around 3h,hydrolysis yield 86.7%,and the purity can reach 96.52%（GC）,98.80% （HPLC）.The synthetic method has the advantage of simplicity of operation,high yield,and high purity.
出处
《宁夏大学学报（自然科学版）》
CAS
2015年第1期56-60,共5页
Journal of Ningxia University(Natural Science Edition)
基金
国家科技支撑计划基金资助项目(2011BAE07B01)
关键词
对乙酰氨基苯磺酰氯
乙胺
N-(4-氨基苯磺酰)-乙胺
医药中间体
p-acetamidobenzene sulfonyl chloride
ethylamine
N-（4-aminobenzene sulfonyl）ethylamine
pharmaceutical intermediates
