化学合成。
医药; 农药
合成路线 1(1. 合成:914358-73-9)
产率:90%
合成条件:With hydrogenchloride; iron In methanol; water for 2 h; Reflux
实验步骤:在40℃下,向工业甲基化酒精(330mL)中的5-溴-2-甲基-3-硝基吡啶(13.8g,63.9mmol)溶液中加入铁粉(20g)(分批以避免结块),然后 用浓盐酸水溶液(5mL)洗脱。 将深棕色混合物在回流下剧烈搅拌2小时,然后冷却并通过Celite过滤。 (用1L工业甲基化酒精洗涤)。 然后真空除去溶剂,将残余物溶于乙酸乙酯(200mL)中,用饱和碳酸氢钠水溶液(200mL)洗涤,用硫酸镁干燥,真空除去溶剂,得到5-溴-2 - 甲基吡啶-3-胺,为橙色固体(10.7g,90%)。 1HNMR(400MHz,CDCl3,δ):7.91(s,1H),7.00(s,1H),3.75(br.s。,2H),2.25(s,3H)。
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