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%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
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)~~
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
dimethyl carbonate
β-cyclodextrin
low substitution degree
methoxycarbonylation
methylation
drug and cosmetic materials
