三甘醇单苄醚在医药和农药领域有应用,具体用途需结合相关研究进一步明确。
医药; 农药
合成路线 1(1. 合成:55489-58-2)
产率:67%
合成条件:Stage #1: With sodium hydroxide In water for 0.17 h; Stage #2: at 100℃;
实验步骤:将三甘醇(30g,0.2mol)溶解在NaOH溶液(8g在8mL H 2 O中)中并搅拌10分钟。 然后加入苄基氯(7mL,0.062mol)并将反应混合物加热至100℃并搅拌过夜。 将粗反应物用饱和NaCl(500mL)稀释,用CH 2 Cl 2(2.x.400mL)洗涤,将有机层用MgSO 4干燥,并蒸发至干。 柱层析(硅胶,乙酸乙酯至乙酸乙酯/ MeOH,10:1),得到淡黄色油状物(9.87g,67%收率)。
参考文献:
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合成路线 2(2. 合成:55489-58-2)
产率:92.9%
:With silver(l) oxide In dichloromethane for 2 h; Inert atmosphere
:将Ag 2 O(6.9g,30mmol)加入到三甘醇(3.0g,20mmol)的无水CH 2 Cl 2溶液中。 然后在5分钟内滴加BnBr(2.6mL,22mmol),并将混合物搅拌2小时。 此后,将悬浮液通过硅藻土垫过滤,将其用CH 2 Cl 2彻底洗涤。 将合并的滤液减压浓缩,并将残余物通过柱色谱纯化,得到黄色油状物(4.46g,92.9%)。 1H NMR(300MHz,CDCl3):δ7.26-7.35(m,5H,Ph),4.56(s,2H,-CH2Ph),3.73-3.58(m,12H,-OCH2CH2O-),2.80(br,1H, -哦); 13 C NMR(75MHz,CDCl 3):δ138.0,128.2,127.6,127.5,73.1,72.4,70.5,70.4,70.2,69.2,61.5。
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