化学合成。
医药; 农药; 染料; 表面活性剂; 橡胶助剂; 饲料添加剂; 食品添加剂; 粘合剂
合成路线 1(1. 合成:3430-21-5)
产率:100%
合成条件:Stage #1: With bromine In dichloromethane at 0 - 20℃; for 4.67 h; Stage #2: With sodium hydroxide In dichloromethane; water
实验步骤:将溴(15.4mL,0.30mol)滴加到搅拌并冷却(0-2 [℃])的2-氨基-3-甲基吡啶(1; 32.44g,0.30mol)的无水[CH 2 Cl 2](1000)溶液中。 mL)在1小时内。 然后除去冷却浴,将黄色悬浮液在室温下搅拌。吨。 持续3小时40分钟。 用2N [NAOH](145mL)将混合物碱化至pH 9,然后用饱和的[NAHCO 3]水溶液(100mL) - 饱和Na 2 S 2 O 3水溶液(10mL)混合物。 分离有机层并用盐水洗涤,干燥[MGSO 4]并浓缩,得到14(56.83g,102%),为棕色固体,将其不经纯化用于下一步骤。
参考文献:
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