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作 者:万玮 彭国颖 顾家 黄喜根[1,2] 黄长干 黄建平 WAN Wei;PENG Guo-ying;GU Jia;HUANG Xi-gen;HUANG Chang-gan;HUANG Jian-ping(College of Science,Jiangxi Agricultural University,Nanchang 330045,China;Nanchang Key Laboratory of Chemical Utilization of Plant Resources,Nanchang 330045,China)
机构地区:[1]江西农业大学理学院,江西南昌330045 [2]南昌市植物资源化学利用重点实验室,江西南昌330045
出 处:《精细化工中间体》2021年第5期70-72,共3页Fine Chemical Intermediates
基 金:国家自然科学基金资助项目(32060703);江西省科技支撑计划项目(20171BBE50027,20202BBEL53028);江西省教育厅科技项目(GJJ170275);南昌市基地和人才计划项目(2018CXTD014)。
摘 要:研究了一种合成三(乙烯醇)单-11-十一烷基硫醇的新方法,即以三乙二醇和1,11-二溴十一烷为底物,经过去质子化、取代、水解3步反应得到目标化合物三(乙烯醇)单-11-十一烷基硫醇。目标产物的总收率为16.5%,其结构经1 H NMR确证。考察了氢化钠用量和水解反应催化剂对产物收率的影响。结果表明,当n(三乙二醇)∶n(氢化钠)=1.00∶1.00时,水解反应催化剂选用浓氨水时,3步反应的收率较高。方法副产物少,污染小,操作简单,适合小批量生产。A novel method for synthesizing triethylene glycol mono-11-mercaptoundecyl ether was studied.Triethylene glycol mono-11-mercaptoundecyl etherwas synthesized through a three-step reaction process includingdeprotonation,substitution and hydrolysis using triethylene glycol and 1,11-dibromoundecane as the starting materials with an overall yield of 16.5%,and its structure was characterized by 1 H NMR.The influence ofthe amount of sodium hydride and the choice of hydrolysis reaction catalyst on the product yield was investigated.The results showed that the yield of the three-step reaction was highest under the conditions includingratio of n(triethylene glycol)to n(sodium hydride)at 1.00∶1.00 and concentrated ammonia as the hydrolysis reaction catalyst.This method has less by-products,simple operation,low pollution,and is suitable for small-batch production.
关 键 词:自组装单层膜 取代反应 三(乙烯醇)单-11-十一烷基硫醇
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