化学合成。
化学合成
合成路线 1(1. 合成:127232-41-1)
产率:86%
合成条件:With lithium aluminium tetrahydride In tetrahydrofuran at 0℃; for 0.50 h;
实验步骤:在0℃下,将33(29.13g,0.207mol)的THF(206mL)溶液滴加到LiAlH 4(7.85g,0.207mmol)的THF(206mL)悬浮液中。 将反应混合物在0℃下搅拌30分钟(此时TLC指示消耗SM)并通过连续加入水(8mL),10%NaOH(8mL)溶液和水(24mL)淬灭。 温度不应超过0°C)。 过滤沉淀物并用THF洗涤数次。 蒸发滤液,得到34,无需纯化即可使用。M =17.7克。产率=86percent。
参考文献:
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