6315-52-2 二对甲苯磺酸乙二醇酯

危险性质：否

路线1（2. 合成：6315-52-2）

• 产率：83%
• 合成条件：at 0 - 20℃; for 2.50 h;
• 实验步骤：将19.8g（0.3mol）乙二醇溶于150ml蒸馏过的吡啶中，然后用冰浴冷却该溶液。在机械搅拌下缓慢加入对甲苯磺酰氯（123g，0.65mol）。添加过程中温度必须保持在20℃以下。当加入约90g时，搅拌变得困难，混合物用200ml吡啶稀释。将反应混合物搅拌2小时30分钟。加入HCl水溶液（12N HCl（170ml）的冰（500ml）溶液）。滤除该添加过程中形成的固体。将该固体溶于回流的甲醇（250ml）中，然后滤除回到室温后形成的新沉淀物。最后，将得到的白色固体真空干燥，得到纯产物（92.4g，收率83％）。特性：1H NMR（200 MHz，CDCl3）δ7.71（d，2H），7.31（d，2H），4.16（s，2H），2.43（s，3H）
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