河南化工
河南化工
하남화공
Henan Chemical Industry
2015年
9期
24-27
,共4页
陈俭%徐珂%张展%崔鹏%田海英%宋成盈
陳儉%徐珂%張展%崔鵬%田海英%宋成盈
진검%서가%장전%최붕%전해영%송성영
酯化%赖氨酸%乙醇%氯化亚砜%赖氨酸乙酯盐酸盐
酯化%賴氨痠%乙醇%氯化亞砜%賴氨痠乙酯鹽痠鹽
지화%뢰안산%을순%록화아풍%뢰안산을지염산염
esterification%lysine%ethanol%dichloride sulfoxide%lysine ethyl ester dihydrochloride
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%。
以賴氨痠和無水乙醇為原料,對賴氨痠乙酯二鹽痠鹽的閤成工藝進行瞭優化。比較瞭不同痠催化劑的影響,髮現在乙醇—氯化亞砜溶液中加入賴氨痠反應,產品分離操作簡單,收率和純度較高。進一步結閤薄層色譜( TLC)和紫外—可見分光光度計( UV-Vis)對反應進程進行鑑控,對氯化亞砜用量、溫度、時間等反應條件進行瞭優化,併通過鎔點測定和傅裏葉變換紅外光譜( FT-IR)分析對產品結構進行瞭確認錶徵。結果錶明:在質量分數30%的氯化亞砜—乙醇溶液中加入賴氨痠,80℃下迴流反應4 h後,賴氨痠乙酯鹽痠鹽分離收率可達95%,產品純度達99%。
이뢰안산화무수을순위원료,대뢰안산을지이염산염적합성공예진행료우화。비교료불동산최화제적영향,발현재을순—록화아풍용액중가입뢰안산반응,산품분리조작간단,수솔화순도교고。진일보결합박층색보( TLC)화자외—가견분광광도계( UV-Vis)대반응진정진행감공,대록화아풍용량、온도、시간등반응조건진행료우화,병통과용점측정화부리협변환홍외광보( FT-IR)분석대산품결구진행료학인표정。결과표명:재질량분수30%적록화아풍—을순용액중가입뢰안산,80℃하회류반응4 h후,뢰안산을지염산염분리수솔가체95%,산품순도체99%。
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%.