摘要
用钾离子为模板,采用稀释法,以三甘醇和3,6-二氧-1,8-二氯辛烷为原料,经Williamson反应合成了18-冠-6,并用硝基甲烷进行提纯。考察了反应时间、反应物配比、氢氧化钾加入方式对产率的影响。实验结果表明:反应时间为20h,三甘醇和三甘醇的二氯化物的物质的量比为1.2∶1,氢氧化钾以粉状加入时,18-冠-6的产率可达51.58％。产物的结构红外光谱及熔点确认。
In dilute solution of aprotic dipolar solvent, using potassium ion as template, 18 - crown - 6 was synthesized by using triethylene glycol and 3,6- dioxa -1,8- dichlorooctane as raw materials, and purified via 18 - crown - 6 -MeNO2 (1:2) complex. The optimum reaction conditions of synthesis are as follows (1) the molar ratio of triethylene glycol to 3,6- dioxa- 1,8- dichlorooctane: 1.2:1; (2) reaction time; 20 hours; (3)potassium hydroxide is powdered. Under the condition the yield of 18 - crown - 6 is 51.58% . The structure was determined by IR and m.p.
出处
《化工时刊》
CAS
1999年第12期18-20,共3页
Chemical Industry Times
