化学合成。
化学合成
合成路线 1(1. 合成:183208-22-2)
产率:100%
合成条件:Stage #1: With sodium hydride In N,N-dimethyl-formamide at 0 - 20℃; Stage #2: at 20℃;
实验步骤:在0℃下,向5-溴-1H-吡咯并[2,3-bjpyndine(1.5g,7.6mmol)的DMF(10mL)溶液中加入NaH(365mg,9.1mmol)。 将混合物在室温下搅拌1.5小时。 加入MeI(1.4g,9.8mmol)并在室温下搅拌过夜。 用饱和NaHCO 3水溶液淬灭反应。 NH 4 Cl溶液(10mL),在水(20mL)和EA(20mL)之间分离。 将有机层用水(10mL)和盐水(10mL)洗涤,经无水Na 2 SO 4干燥。 除去溶剂,得到5-溴-1-甲基-1H-吡咯并[2,3-bjpyndine(1.7g,收率:定量),为浅黄色晶体。 'HNMR(300 MHz,CDC13):= 8.34(d,J = 2.1 Hz,1H),8.01(d,J 2.4 Hz,1H),7.18(d,J = 3.6 Hz,1H),6.39(d,J = 3.3Hz,1H),3.86(s,3H)。
参考文献:
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