碱液中单6-对甲苯磺酰酯-β-环糊精的制备

摘要

以β-环糊精(β-CD)与对甲苯磺酰氯(p-TsCl)为原料,在不加入有机溶剂的条件下,采用分批加料的方式,在氢氧化钠溶液中制备了单6-对甲苯磺酰酯-β-环糊精(6-OTs-β-CD).通过单因素法考察了反应条件对目标产物收率的影响,得到的较佳工艺条件为:反应温度为0℃,反应时间为5h,碱液浓度为0.45 mol/L,n(p-TsCl):n(β-CD)＝4,碱液用量为240 mL(β-CD的加入量为8 g时).在较佳工艺条件下,6-OTs-β-CD的收率可达46.2％.%Adopting batch feeding, 6-deoxy-tosyl-β-Cyclodextrin(6-Ots-β-CD) was prepared by batch-wise feeding of β-cyclodextrin(β-CD) and p-toluene sulfonyl chloride (p-TsCl) in sodium hydroxide a-queous solution without the introduction of organic reagents. By examining effects of reaction conditions on the yield with single-factor method, the optimum technological conditions were found as follows: reaction temperature 0 ℃ , total reaction time 5 h, alkali solubility 0.45 mol/L, n(p-TsCl) :n (β-CD) = 4, the amount of alkali solution 240 mL(when the amount of β-CD is 8 g ). Under these conditions, the yield of 6-Ots-β-CD is up to 46. 2%.