化学合成。
化学合成
合成路线 1（1. 合成：87184-99-4）
产率：95%
合成条件：Stage #1: With 1H-imidazole In dichloromethane at 0℃; for 0.50 h; Inert atmosphere Stage #2: at 0 - 20℃; for 1 h; Inert atmosphere
实验步骤：在0℃下向搅拌的丁-1,4-二醇（3mL，33.3mmol）的无水CH 2 Cl 2（30mL）溶液中加入咪唑（2.73g，66.6mmol）并将混合物搅拌30分钟。 加入溶解在CH 2 Cl 2（20mL）中的TBSCl（5g，33.3mmol）并将混合物在室温下搅拌。 持续1小时（TLC监测）。 将混合物用饱和NaHCO 3淬灭。 用NH 4 Cl溶液萃取，用CH 2 Cl 2（2×30mL）萃取。 将合并的有机萃取液用盐水洗涤，干燥（Na 2 SO 4），并真空浓缩。 通过柱色谱（硅胶，EtOAc-己烷，2：8）纯化残余物，得到TBS醚2，为无色浆状物; 产量：6.4克（95％）。
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合成路线 2（3. 合成：87184-99-4）
产率：88%
合成条件：With 1,11-bis(3-methyl-3H-imidazolium-1-yl)-3,6,9-trioxaundecane di(methanesulfonate) In methanol at 20℃; for 1.50 h;
实验步骤：通用程序：将TBDMS醚（1.0mmol）和[tetraEG（mim）2] [OMs] 2 IL（0.2mmol）在甲醇（4mL）中的混合物在室温下搅拌直至反应完成。 通过薄层色谱（TLC）监测反应进程。 反应完成后，减压除去甲醇，残余物用乙醚萃取并经硫酸钠干燥。 减压蒸发乙醚，得到各自的产物。
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