超声法合成D-葡萄糖酸-δ-内酯  

Synthesis of D-glucose Acid-δ-lactone Through Ultrasonic Method

作　　者：王丽艳[1] 范琳琳[1] 孙竹[1] 邢凤兰[1] 赵冰[1] 

机构地区：[1]齐齐哈尔大学化学与化学工程学院,黑龙江齐齐哈尔101006

出　　处：《化学世界》2013年第5期305-307,共3页Chemical World

基　　金：黑龙江省教育厅科学技术项目(12511591)

摘　　要：研究了连续性超声反应条件下D-葡萄糖酸-δ-内酯合成的新方法。考察了反应时间、反应温度、葡萄糖与I2的摩尔比对反应的影响。经过正交试验确定了较佳的合成工艺条件为:n(葡萄糖)∶n(I2)=1∶2,40℃下连续超声反应40min,生成的葡萄糖酸钾收率为93%,将其水溶液经过强酸性苯乙烯系阳离子交换树脂柱,酸液在45℃下减压浓缩,20℃下静置过夜重结晶得到D-葡萄糖酸-δ-内酯,收率88%,产物通过IR,1 H NMR得到证实。结果表明,连续性超声反应合成D-葡萄糖酸-δ-内酯,操作简单,反应时间短,收率高。D-Glucose acid-δ-lactone was synthesized from glucose and iodine by continuous ultrasonic irradiation.The influence of reaction time,reaction temperature and molar ratio of glucose to iodine were investigated.The optimum process conditions were determined through orthogonal design as follows：the molar ratio of glucose to iodine was 1∶2,the reaction temperature was 40℃,the reaction time was 40 min.The yield of potassium gluconate was 93%.Then the potassium gluconate aqueous solution was passed through a column of strong acid cation exchange resin of styrene.The acidic liquor was collected and concentrated by rotary evaporator at 45℃.After recrystallization overnight at 20℃,the yield of D-glucose acid-δ-lactone was 88%.The product structure was confirmed by IR,1H NMR.The results show that the continuous ultrasonic reaction promotes the synthesis of D-glucose acid-δ-lactone with simple operation,short reaction time,and high yield.

关 键 词：D-葡萄糖酸-δ-内酯 连续性超声法 合成 表征 

分 类 号：TQ921[轻工技术与工程—发酵工程]