单6-(3-乙氧基-2-羟基)丙基-β-环糊精的合成  

Synthesis of Mono 6-(3-ethoxy-2-Hydroxy)propyl-β-Cyclodextrin

作　　者：张毅民[1] 甘永江[1] 张国栋[1] 王虹[1] 苑珊[1] 

机构地区：[1]天津大学绿色合成与转化教育部重点实验室,天津300072

出　　处：《天津理工大学学报》2007年第3期60-63,79,共5页Journal of Tianjin University of Technology

摘　　要：以无水乙醇和环氧氯丙烷为原料在相转移催化剂存在条件下合成了乙基缩水甘油醚,用乙基缩水甘油醚和β-环糊精为原料,在30%(w/w)的氢氧化钠水溶液中合成了6-(3-乙氧基-2-羟基)丙基-β-环糊精.通过薄层色谱研究发现,展开剂正丙醇:水:氨水=6:3:1(V/V)能有效分离6-(3-乙氧基-2-羟基)丙基-β-环糊精,经柱层色谱分离得到单6位取代和多取代的(3-乙氧基-2-羟基)丙基-β-环糊精,反应的收率分别为14%和6.5%.利用红外光谱、差热扫描量热分析、质谱和核磁共振技术对所合成的产品进行了表征.Ethyl glycidyl ether （EGE） was obtained from ethyl alcohol and epichlorohydrin by phase-transfer catalysis methodology. Using synthesized EGE and β-cyclodextrin as raw materials, 6-（3-ethoxy-2-hydroxy）propyl-β-cyclodextrins were obtained in 30% （w/w） concentration of sodium hydroxide. Through studying TLC, a kind of the effective developing solvent of 1-propanol： water： concd aq ammonia （6：3：1 ,V/V） can successfully separate crude product, and silic gel column chromatography was used to purify crude product to get mono and heptakis 6-（3-ethoxy-2-hydroxy） propyl-β-cyclodextrins in yields of 14% and 6.5%, respectively. Their structures were verified by IR, DSC, MS, ^1HNMR and ^13CNMR instruments.

关 键 词：Β-环糊精 乙基缩水甘油醚 核磁共振 薄层色谱 柱色谱 

分 类 号：O621.3[理学—有机化学]