摘要
以1,3-丙二胺为起始原料,经过5步反应,得到2-[{3-[双(2-羟乙基)氨基]丙基}(十八烷基)氨基]乙醇二氢氟化物,简称奥拉氟。氨基保护反应的较优条件为:选择乙酸乙酯作为反应溶剂,0℃下滴加二碳酸二叔丁酯3h,反应温度为室温,中间体Ⅱ的产率可达97.4%。烷基化反应的最优反应温度为80℃,中间体Ⅲ的产率可达88.1%。脱保护时选择4mol·L^(-1)盐酸进行反应,搅拌过夜得到中间体Ⅳ。在羟乙基化反应中,底物与环氧乙烷的摩尔比为1∶5时,中间体Ⅴ的产率可达70.2%。中间体Ⅴ与HF发生成盐反应得到目标产品Ⅰ。产物经Micro-LC、FTIR、^(1)HNMR和^(13)CNMR进行了表征。
Applied 1,3-propanediamine as the starting material,after 5 steps of reaction,2-[{3-[bis(2-hydroxyethyl)amino]propyl}(octadecyl)amino]ethanol dihydrofluoride was obtained,commonly known as olafluoride.Among them,the optimal conditions for the amino protection reaction were as followed:ethyl acetate was selected as the reaction solvent,di-tert-butyl dicarbonate was added dropwise at 0℃for 3h,the reaction temperature was room temperature,and the yield of intermediateⅡreached 97.4%.The optimal reaction temperature of alkylation reaction was 80℃,and the yield of intermediateⅢreached 88.1%.4 mol/L hydrochloric acid was selected for the reaction,and intermediateⅣwas obtained by stirring overnight.When the molar ratio of substrate to ethylene oxide in the hydroxyethylation reaction is 1:5,the yield of intermediateⅤreach 70.2%.The target productⅠwas obtained by HF salting.The products were characterized by Micro-LC,FTIR,^(1)HNMR and ^(13)CNMR.
作者
杨佳
柯建学
方林
廖振
梁阳
邱黎
刘小成
邓嘉伦
YANG Jia;KE Jianxue;FANG Lin;LIAO Zhen;LIANG Yang;QIU Li;LIU Xiaocheng;DENG Jialun(Hubei Research Institute of Chemistry,Jianghan University,Wuhan 430056,China;Haiso Technology Co.,Ltd.,Wuhan 430074,China)
出处
《化工技术与开发》
2025年第10期22-26,共5页
Technology & Development of Chemical Industry
关键词
1
3-丙二胺
奥拉氟
产率
表征
1,3-propanediamine
olafur
yield
characterization
