化学合成。
化学合成
合成路线 1(1. 合成:443956-08-9)
产率:96%
合成条件:With bromine; sodium methylate In methanol at 0 - 20℃; for 1 h;
实验步骤:将3-羟基-2-硝基吡啶(20g,0.143mol)溶解在甲醇(400mL)中,在室温下加入25%甲醇钠的甲醇溶液(33mL,0.13mol)。 将混合物搅拌30分钟,然后冷却至0℃,缓慢加入溴(7.2mL,0.14mol)。 将反应在0℃搅拌30分钟,然后用冰AcOH(2.5mL)淬灭。 真空除去溶剂,得到物质(30g,96%),其无需进一步纯化即可使用:MS(ES)m / z219.0(M + H)+。
参考文献:
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