化学合成。
化学合成
合成路线 1(1. 合成:34595-26-1)
产率:92%
合成条件:With potassium carbonate In DMF (N,N-dimethyl-formamide) at 130℃; for 3 h;
实验步骤:向醛3a(20g,161.1mmol)的无水DMF(160ml)溶液中依次加入哌啶(19.1ml,193.4mmol,1.2当量)和碳酸钾(26.73g,193.4mmol,1.2当量)。 将悬浮液在130℃下加热3小时。 然后将反应混合物倒入冷水中。 用柠檬酸酸化至pH5。将水层用EtOAc萃取3次,并将合并的有机萃取物依次用水,饱和NaHCO3和盐水洗涤。 用MgSO 4干燥有机萃取物,过滤并浓缩,分离出所需的2-哌啶子基苯甲醛3b,为红色油状物(28.23g,收率92%)。
参考文献:
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