微波辅助合成甲氧羰基-β-环糊精碳酸酯  

Microwave-Assisted Synthesis of Methoxycarbonyl-β-Cyclodextrin Carbonate

作　　者：张毅民[1] 刘红莎[1] 张惠莹[1] 朱艳芳[2] 

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 [2]天津大学管理与经济学部,天津300072

出　　处：《化学工业与工程》2014年第4期36-40,79,共6页Chemical Industry and Engineering

基　　金：濮阳市科技局资助项目(080527)

摘　　要：以绿色试剂碳酸二甲酯、β-环糊精为原料,无水碳酸钾为催化剂,探索了在N,N-二甲基甲酰胺溶剂中,采用微波辐射技术一步合成甲氧羰基-β-环糊精碳酸酯的新工艺。采用红外光谱、核磁共振技术对产品结构进行了表征,红外谱图在1 751 cm-1处有典型的C O峰,13C-NMR核磁谱证明有碳酸酯C O及CH3O—,由此推测其结构为β-CD-OCOOCH3。应用电喷雾质谱测定了产品平均取代度为2.423,并结合高效液相色谱法测定了原料β-环糊精转化率为93.22%。结果表明:该新工艺合成了一种新型化合物β-环糊精碳酸酯,而且与传统合成工艺相比,其具有能耗低,收率高,反应时间短等优点。A novel microwave-assisted procedure for the synthesis of methoxycarbonyl-β-cyclodextrin carbonate is described in the work.Methoxycarbonyl-β-cyclodextrin carbonate was obtained through reaction of green reagent dimethyl carbonate and β-cyclodextrin with anhydrous potassium carbonate as catalyst in N,N-dimethylformamide under microwave radiation.The structure of the product was characterized by IR and13C-NMR.A typical C O peak at 1 751 cm-1in IR spectrum and13C-NMR signal of C O and CH3O— indicated distinctly the structure of β-CD-OCOOCH3.The average degree of substitution of the products and the raw material conversion are 2.423 and 93.22%,respectively,determined by electrospray mass spectrometry and high performance liquid chromatographic.The experimental results showed that the novel process for the synthesis of β-cyclodextrin carbonate,compared with the conventional heating process,has the advantages of low energy consumption,high yield and short reaction time,etc.

关 键 词：微波辐射 碳酸二甲酯 取代度 β-环糊精碳酸酯 

分 类 号：O621.3[理学—有机化学]