摘要
以羟乙基磺酸钠为原料,与氯化亚砜反应制备2-氯乙基磺酰氯;然后采用2-氯乙基磺酰氯与邻苯二甲酰亚胺钾盐反应制备N-(2-邻苯二甲酰亚氨基乙磺酰基)邻苯二甲酰亚胺(中间体1);中间体1经硼氢化钠还原、盐酸酸化得到2-氨基乙基磺酰胺盐酸盐,总收率为80.26%,与文献报道方法相比总收率提高了33.34%。通过熔点、红外光谱、气相色谱-质谱联用、高分辨质谱和核磁共振氢谱对中间体和产品进行了表征。
The 2-aminoethanesulfonamide was synthesized from commercially available sodium isethionate as raw materials in three steps and 80. 26% total yield. The 2-chloroethanesulfonyl chloride was preparated using sodium isethionate by chlorination with thio- nyl dichloride,and the 2-chloroethanesulfonyl chloride was transformed into the intermediate 1 with potassium phthalimide for the first time. The reduction reaction was carried out in ethanol with NaBH4 as reductants. The structure of 2-aminoethanesulfonamide was confirmed by IR,melting point GC-MS and 1H - N M R .
出处
《化学研究与应用》
CSCD
北大核心
2017年第5期733-735,共3页
Chemical Research and Application
基金
河南省重点科技攻关计划项目(152102210162)资助