不同温度下碳酸二甲酯对β-环糊精的改性研究  

Modification of β-Cyclodextrin with Dimethyl Carbonate at Different Temperature

作　　者：张毅民[1] 张惠莹[1] 刘红莎[1] 黄德超[1] 

机构地区：[1]天津大学化工学院绿色合成与转化教育部重点实验室,天津300072

出　　处：《精细化工》2013年第5期544-548,共5页Fine Chemicals

基　　金：濮阳市科技局资助项目(080527)~~

摘　　要：以碳酸二甲酯和β-环糊精为原料,以无水碳酸钾为催化剂,在N,N-二甲基甲酰胺介质中,考察了常压和高压条件下温度在50～170℃碳酸二甲酯对β-环糊精的改性作用。所得产品用制备型高效液相色谱分离纯化,用红外光谱、质谱和核磁共振光谱进行了表征。结果表明,在50～85℃,发生的是低取代的甲氧羰基化反应;在90～140℃,甲氧羰基化和甲基化反应均有发生;在160～170℃,压力约为1.40 MPa时,主要反应产物为取代度为7～9的随意甲基化β-环糊精,且收率达80%～85%。The modification effect of β-cyclodextrin by dimethyl carbonate in the temperature range of 50 % to 170 % was systematically studied at atmospheric and high pressure respectively, using dimethyl carbonate as green modification reagent and anhydrous potassium carbonate as alkaline catalyst in N, N-dirnethylformamide. The products were purified through preparative HPLC, and characterized by means of IR, ESI-MS,1HNMR and 13CNMR. The results show that methoxycarbonylation derivatives with low degree of substitution were prepared in the temperature range of 50 ℃ to 85 ℃ ;the methylation and methoxycarbonylation of 13-cyclodextrin occurred simultaneously in the range of 90 % to 140 ℃;when operating at the temperature from 160 ℃ to 170 ℃ ,and at the pressure of approximately 1.40 MPa, random methylated/3-cyclodextrins with the substitution degree range of 7 to 9 were obtained with a high yield of 80% to 85%.

关 键 词：碳酸二甲酯 Β-环糊精 低取代度 甲氧羰基化 甲基化 医药与日化原料 

分 类 号：O636.12[理学—高分子化学]