化学合成。
化学合成
合成路线 1(1. 合成:77893-68-6)
产率:100%
合成条件:With N-Bromosuccinimide; acetic acid In chloroform for 1.50 h; Reflux
实验步骤:化合物28-1(0457)向3-氯噻吩(6.52g,55mmol)的CHCl 3(30mL)和AcOH(30mL)溶液中加入NBS(9.80g,55mmol)。 将混合物在回流下加热1.5小时,然后冷却至室温。 加入水(70mL)并将混合物用CHCl 3(30mL×2)萃取。 将合并的有机层用饱和NaHCO 3洗涤。 NaHCO 3(40mL)和盐水(30mL),经无水Na 2 SO 4干燥,过滤,浓缩,得到28-1,为棕色油状物(10.02g,定量收率),其直接用于下一步骤。
参考文献:
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