化学合成。
医药
合成路线 1(1. 合成:158407-04-6)
产率:94%
合成条件:With carbon tetrabromide; triphenylphosphine In dichloromethane at 0 - 20℃; for 22 h;
实验步骤:化合物14; 将EPO N-BOC哌啶-4-甲醇(1g; 46.5mmol)和四溴化碳(1.7g; 51.3mmol)溶解在二氯甲烷(20ml)中并冷却至0℃。 加入三苯基膦(0.98g; 37.3mmol)并将反应在室温下搅拌16小时。 加入另外的三苯基膦(0.4g; 15.7mmol)和四溴化碳(0.24g; 7.2mmol)并继续搅拌6小时。 蒸发溶剂并将残余物在二氧化硅上进行色谱分离。 用20%乙酸乙酯的庚烷溶液(1.22g,94%)洗脱N-BOC哌啶-4-甲基溴。
参考文献:
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