化学合成,作为结构单元用于高效钯催化合成2-吡啶基氮杂薁,这是一种表现出pH和阳离子金属依赖性发射光谱的双齿配体。
化学合成
合成路线 1(1. 合成:17997-47-6)
产率:100%
合成条件:Stage #1: With n-butyllithium In tetrahydrofuran at -70℃; for 0.50 h; Inert atmosphere Stage #2: at -70℃; for 2 h;
实验步骤:向2-溴吡啶(XCVI)(10g,63mmol,1.00当量)的THF(150mL)溶液中加入n-BuLi(25.3mL,63mmol,1.00当量),并将混合物在-70°搅拌 在氮气氛下30分钟。 然后加入n-Bu 3 SnCl(21.7g,67mmol,1.06当量),将混合物在相同温度下再搅拌2小时。 向溶液中加入饱和氯化铵溶液(150mL),用乙酸乙酯(150mL×3)萃取。 将合并的有机层用Na 2 SO 4干燥,过滤并真空浓缩,得到粗制2-(三丁基甲锡烷基)吡啶(XCVII)(25.9g,63mmol,100%收率),为黄色油状物。 粗产物无需进一步纯化即可使用。
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