Microwave-Assisted Synthesis of Methoxycarbonyl-β-Cyclodextrin Carbonate
ZHANG Yi-Min1, LIU Hong-Sha1, ZHANG Hui-Ying1, ZHU Yan-Fang2
(1.School of Chemical Engineering and Technology, Tianjin University, Key Laboratory for Green Chemical Technology ofMinistry of Education, Tianjin 300072, China; 2. Department of Management and Economics, Tianjin University, Tianjin 300072, China)
Abstract 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 and 13C-NMR. A typical CO peak at 1 751 cm-1 in IR spectrum and 13C-NMR signal of CO 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.
ZHANG Yi-Min, LIU Hong-Sha, ZHANG Hui-Ying, ZHU Yan-Fang.Microwave-Assisted Synthesis of Methoxycarbonyl-β-Cyclodextrin Carbonate[J] Chemcial Industry and Engineering, 2014,V31(4): 36-40