化学合成。
化学合成
合成路线 1(1. 合成:33421-36-2)
产率:75%
合成条件:With oxone; Ru(MesCO 2 )(4,4'-dibromobipyridine)(p-cymene); trifluoroacetic acid; trifluoroacetic anhydride In 1,2-dichloro-ethane at 140℃; for 8 h; Sealed tube; Green chemistry
实验步骤:通用方法:2-芳基吡啶(1当量),Ru(MesCO2)(L)(对伞花烃)[L-2,2'-吡啶或4,4'-二溴联吡啶](5mol%)的混合物,TFA: TFAA = 0.6ml:0.4ml,将Oxone(4eq)置于30ml密封管中。 加入1ml DCE,然后将管置于油浴中,搅拌,并在140℃下加热。 每8小时检查反应进程。 在原料完全消耗后,将反应混合物冷却至室温,用盐水淬灭并用二氯甲烷萃取。 将合并的有机层用无水Na 2 SO 4干燥,并真空蒸发。 通过硅胶柱(洗脱液:己烷/乙酸乙酯)纯化粗产物,得到所需产物。
参考文献:
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