| 张毅民,徐景娜,白家瑞.化学通报,2017,80(6):585-588,572. |
| 磺丁基醚-β-环糊精的微波辅助合成及结构表征 |
| Microwave-Assisted Synthesis and Characteration of Sulfobutyl Ether β-Cyclodextrins |
| 投稿时间：2016-10-22 修订日期：2016-12-25 |
| DOI： |
| 中文关键词: β-环糊精 1,4丁磺内酯 磺丁基醚-β-环糊精 微波辐射 |
| 英文关键词:β-cyclodextrin 1,4-butane sultone sulfobutyl ether-β-cyclodextrins microwave radiation |
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| 中文摘要: |
| 以1,4丁磺内酯、β-环糊精为原料,采用微波辐射加热及分步碱的方法,探究了合成不同取代度磺丁基醚-β-环糊精的新工艺,并考察了初始加碱量对产物取代度的影响。合成工艺条件为：β-环糊精与1,4丁磺内酯的摩尔比分别为：1:1.1, 1:4, 1:8,反应温度为85℃,微波输出功率为400W。该条件下,反应时间2～3h,所得产品的平均取代度分别为1.12, 3.96, 6.83,收率达85%。采用红外、核磁共振、质谱和毛细管电泳技术对合成的产品进行结构表征及取代度计算。实验结果表明：该新工艺合成了特定取代度的磺丁基醚-β-环糊精,而且与传统合成工艺相比,具有反应时间短、用碱量少、反应条件温和等优点。 |
| 英文摘要: |
| A novel microwave-assisted synthesis of sulfobutyl ether-β-cyclodextrins were investigated through reaction between β-cyclodextrin and 1,4-butane sultone with adding the alkali stepwise. The effects of initial amount of alkali on the degree of substitution were evaluated. Synthesis conditions: the molar ratios of 1,4-butane sultone and β-cyclodextrin sultone are: 1:1.2, 1:5, 1:8, respectively, the reaction temperature is 85℃, microwave output power is 400W. Under these conditions, the reaction time is 2h to 3h, the average degrees of substitution of products are 1.12, 3.96, 6.83, separately, and the maximum yield of sulfobutyl ether β-cyclodextrin derivatives is up to 85%. The average degree of substitution and the characterization of sulfobutyl ether β-cyclodextrin derivatives were investigated by means of IR, 1H NMR, 13C- NMR, MS and Capillary Electrophoresis. The experimental results show that the novel process for the synthesis of sulfobutyl ether β-cyclodextrin derivatives with specific average degree of substitution, compared with the conventional heating process, has the advantages of short reaction time, less alkali, moderate reaction condition, etc. |
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