化学合成;生命科学。
化学合成;生命科学
合成路线 1(1. 合成:56926-94-4)
产率:91%
合成条件:at 0℃; for 8 h; Inert atmosphere
实验步骤:向在冰浴上冷却的5(0.67g,3.1mmol)的吡啶(10mL)溶液中加入对甲苯磺酰氯(3.0g,15.7mmol)。 在氮气氛下在冰浴上搅拌8小时,向溶液中加入Et 2 O(10mL),并将混合物在室温下进一步搅拌14小时。 将得到的黄色溶液用水,10%硫酸氢钾,饱和碳酸氢钠和盐水洗涤。 将醚层用MgSO 4干燥并蒸发。 通过硅胶柱色谱法(己烷:EtOAc = 2:1)纯化获得的无色油状物,得到6,为白色固体(1.05g,91%)。 6的光谱数据与文献相同.32纯度通过1H NMR确认。
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