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作 者:陈俭[1] 徐珂[2] 张展 崔鹏[1] 田海英 宋成盈[1]
机构地区:[1]郑州大学化工与能源学院,河南郑州450001 [2]中国烟草总公司职工进修学院,河南郑州450008 [3]河南中烟工业有限责任公司,河南郑州450000
出 处:《河南化工》2015年第9期24-27,共4页Henan Chemical Industry
摘 要:以赖氨酸和无水乙醇为原料,对赖氨酸乙酯二盐酸盐的合成工艺进行了优化。比较了不同酸催化剂的影响,发现在乙醇—氯化亚砜溶液中加入赖氨酸反应,产品分离操作简单,收率和纯度较高。进一步结合薄层色谱(TLC)和紫外—可见分光光度计(UV-Vis)对反应进程进行监控,对氯化亚砜用量、温度、时间等反应条件进行了优化,并通过熔点测定和傅里叶变换红外光谱(FT-IR)分析对产品结构进行了确认表征。结果表明:在质量分数30%的氯化亚砜—乙醇溶液中加入赖氨酸,80℃下回流反应4 h后,赖氨酸乙酯盐酸盐分离收率可达95%,产品纯度达99%。Using lysine and anhydrous ethanol as raw materials ,the synthesis process of lysine ethyl ester dihydrochloride is optimized .The influence of different acid catalysts are compared .It is found that when lysine is added to ethanol -dichloride sulfoxide solution ,the product can be simply separated with a high yield and purity.Furthermore, thin layer chromatography (TLC) and ultraviolet-visible spectrophotome-ter ( UV-Vis) is used to monitor the reaction process .Other reaction conditions such as the dosage of di-chloride sulfoxide ,temperature and time are also optimized .The structure of the product is confirmed by fourier transform infrared spectroscopy ( FT-IR ) analysis and melting pointis is determinaed .Results show that when lysine are added into 30%dichloride sulfoxide ethanol solution ,refluxed for 4 h under 80℃,the separated yield of lysine ethyl ester dihydrochloride reached 95%,and the product purity is up to 99%.
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