4-甲基胍基丁酸的合成研究 |
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引用本文: | 韦鹏,郭睿,孙江,来肖,赵艳艳,孙靖.4-甲基胍基丁酸的合成研究[J].安徽农业科学,2010,38(23):12550-12551,12553. |
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作者姓名: | 韦鹏 郭睿 孙江 来肖 赵艳艳 孙靖 |
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作者单位: | 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 |
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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。
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关 键 词: | 胍类 杀菌剂 N-甲基吡咯烷酮 盐酸 二氧化硫脲 |
Study on Synthesis of 4-(methylamino)butanoic Acid |
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Institution: | WEI Peng et al (Key Laboratory of Auxiliary Chemistry and Technology in Light Industry,Ministry of Education,Shaanxi University of Science & Technology,Xi'an,Shaanxi 710021) |
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Abstract: | 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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Keywords: | Guanidine Antiseptic N-methylpyrrolidone Hydrochloric acid Thiourea dioxide |
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