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机构地区:[1]渭南师范学院化学与生命科学学院,渭南714000
出 处:《科学技术与工程》2013年第30期8983-8985,8994,共4页Science Technology and Engineering
基 金:渭南师范学院(12YKSO18)资助
摘 要:研究了以2-噻吩乙胺和甲醛为原料聚合反应得到N-(2-噻吩乙基)亚甲胺,并在乙醇氯化氢的作用下环合得到4,5,6,7-四氢噻吩并[3,2-c]吡啶盐酸盐(HPLC)的工艺过程.讨论了溶剂、酸浓度、反应时间、反应温度对合成的影响.获得最佳反应条件是:酸为30%无水乙醇氯化氢溶液,反应溶剂为乙醇,反应时间控制在3~5h,反应温度是50~ 60 ℃,优化后两步总产率约87%,HPLC含量在99%左右.N-(2-ethyl) thiophene methylamine was prepared through polymerization reaction using 2-Thiopheneethylamine and formaldehyde as the raw materials.Then 4,5,6,7-Tetrahydrothieno [3,2,c] pyridine hydrochloride prepared through cyclization reaction in the presence of ethylalcohol and hydrogen chloride.The effect of solvent and acid concentration,reaction time,reaction temperature on the synthesis were studied discussed.The best reaction conditions were that acid is in the 30% absolute ethyl alcohol and hydrogen chloride solution,the reaction solvent is ethanol,reaction time carried out for 3 to 5 hours,the reaction temperature is 50 ~ 60 ℃,the optimized two overall yield of about 87%,the content of HPLC is about 99%.
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