三甘醇二对甲苯磺酸酯作为有机合成中间体,在医药研发及相关有机化学反应中发挥作用,用于构建特定分子结构。
医药; 有机合成
合成路线 1(1. 合成:19249-03-7)
产率:99%
合成条件:With potassium hydroxide In dichloromethane at 0 - 10℃; for 3 h;
实验步骤:通用方法:化合物2a-c通过文献1中已知的改进方法制备。 将低聚乙二醇(37.7mmol)和对甲苯磺酰氯(14.4g,75.4mmol,2当量)溶解在二氯甲烷(36mL)中,将该溶液冷却至0℃。 在永久搅拌期间,加入研磨的氢氧化钾(17g,302mmol,8当量),然后将溶液搅拌3小时,同时将温度保持在0至10℃。 通过TLC(UV检测)监测该反应。 升温至室温后,将反应混合物用氯仿稀释,用水(3×1:1)萃取。 收集氯仿萃取物,用硫酸镁干燥过夜,过滤并减压蒸发溶剂。
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