摘要
2-氯咪唑并[1,2-α]吡啶-3-磺酰胺是合成低毒长效除草剂咪唑黄隆的重要中间体,以2-氯咪唑并[1,2-α]吡啶为起始原料,采用氯磺酸磺化法合成了2-氯咪唑并[1,2-α]吡啶-3-磺酰胺.采用单因素法优化了实验条件,并利用傅立叶变换红外光谱仪(FT IR)和质谱仪(M S)等手段对产物的结构进行了分析和表征.实验结果表明,磺酰化反应的最佳反应时间为4 h,氯磺酸与2-氯咪唑并[1,2-α]吡啶的用量比为1.2¨1,加入三乙胺可将收率由15.4%提高到70%以上;氨解反应的最佳反应时间为3 h,反应温度为27℃,加入乙腈可将收率由60.1%提高到79.6%;方案经改进后,总反应时间缩短3 h,收率提高了5.5%.
2-Chloroimidazo[1,2-α]pyridine-3-sulfonamide is the most important intermediate for synthesizing low toxicity herbicide imazosulfuron. The synthesis of 2-chloroimidazo [ 1, 2-α] pyridine-3-sulfonamide was investigated. 2-chloroimidazo [1, 2-α] pyridine.-3-sulfonamide was prepared with chlorosulfonic acid and 2-chloroimidazo[1,2-α]pyridine. The experiment condition was explored and optimized, and the products were characterized by FTIR, MS, etc. The results indicate that the optimized sulfonylation reaction time is 4 h, the materiel rate of chlorosulfonic acid and 2-chloroimidazo[1,2-α]pyridine is 1.2 ： 1, with ethylamine the yield increasing from 15.4% to above 70%; the optimized ammonolysis reaction time is 3 h and the reaction temperature is 27℃, with the acetonitrile yield increasing from 60.1% to above 79.6%. After the improvement of the scheme, the total reaction time is reduced by 3 h and the yield is increased by 5.5 %.
出处
《中国矿业大学学报》
EI
CAS
CSCD
北大核心
2005年第6期804-807,共4页
Journal of China University of Mining & Technology
基金
江苏省高校高新技术产业化项目(JH02-093)
