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作 者:韦鹏[1] 郭睿[1] 孙江[1] 来肖[1] 赵艳艳[1] 孙靖
机构地区:[1]陕西科技大学,教育部轻化工助剂化学与技术重点实验室,陕西西安710021 [2]西安三业精细化工有限责任公司,陕西西安710075
出 处:《安徽农业科学》2010年第23期12550-12551,12553,共3页Journal of Anhui Agricultural Sciences
摘 要:以N-甲基吡咯烷酮、盐酸、二氧化硫脲为原料,经2步反应合成4-甲基胍基丁酸。第1步最佳合成条件为:n(N-甲基吡咯烷酮):n(HCl10%)=1∶2.0,反应温度135℃,反应时间5h,此时中间体4-甲基氨基丁酸盐酸盐的收率为72.89%。第2步最佳合成条件为:n(4-甲基氨基丁酸盐酸盐):n(二氧化硫脲)=1∶1.20、反应温度25℃、反应时间12h,此时目标产物的收率为82.68%。用傅立叶变换红外光谱、元素分析对中间体和目标产物进行了结构表征。The 4-(methylamino)butanoic acid was synthesised with N-methyl-pyrrolidone,hydrochloric acid,thiourea dioxide as materials. Under the optimized reaction conditions for 4-(methylamino) butanoic acid salts synthesis:n (N-methyl pyrrolidone):n (HCl 10%) = 1:2.0,reaction temperature 135 ℃,reaction time 5 h,then the yield of intermediate 4-(methylamino)butanoic acid salts was 72.89%. The 4-methylguanidine butyric acid was obtained by reacting the intermediate with thiourea dioxide. Under the optimized reaction conditions for 4-methylguanidine butyric acid synthesis:n (4-methyl-butyric acid salt of ammonia salts):n (thiourea dioxide) = 1:1.20,reaction temperature 25 ℃,reaction time 12 h,then the target product was 82.68%. Both the intermediate and target product was characterized by means of FTIR,EA.
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