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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加碱的方法,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。合成工艺条件是: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,反应时间2~3h。该条件下所得产品的平均取代度分别为1.12、3.96、6.83,收率分别为86.3%、85.6%、85.1%。采用红外、核磁氢谱、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。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。
Using 1,4-butane sultone and β-cyclodextrin as raw materials, the new technology of synthesizing sulfobutylether-β-cyclodextrin with different degree of substitution was explored by microwave heating and step-wise addition of alkali The effect of initial alkalinity on product substitution degree was investigated. The synthesis conditions are as follows: the molar ratio of β-cyclodextrin to 1, 4-butane sultone is 1: 1.1, 1: 4 and 1: 8 respectively, the reaction temperature is 85 ℃, the microwave output power is 400W, the reaction time 2 ~ 3h. Under these conditions, the average degree of substitution of the products obtained was 1.12, 3.96 and 6.83, respectively, and the yields were 86.3%, 85.6% and 85.1% respectively. The synthesized products were characterized by IR, 1H-NMR, MS and capillary electrophoresis. The results show that the new technology synthesizes sulfobutyl ether-β-cyclodextrin with specific degree of substitution, and has the advantages of short reaction time, less alkali dosage and mild reaction conditions compared with the traditional synthesis process.