医药; 农药; 化学试剂; 精细化学品; 药物研发
合成路线 1(1. 合成:4926-28-7)
产率:86%
合成条件:Stage #1: With hydrogen bromide; bromine In water at -20 - -15℃; for 3 h; Stage #2: With sodium nitrite In water at 20℃; for 3 h; Stage #3: With sodium hydroxide In water at 0℃;
实验步骤:在-20℃下向2-氨基-4-甲基吡啶(120g,1.1mol)在48%HBr(1.5L)中的溶液中逐滴加入溴(160mL,3.11mol)。 将反应混合物在-15℃至-20℃搅拌3小时。向上述混合物中分批加入NaNO 2水溶液(204g,2.95mol)。 然后将反应混合物在3小时内温热至室温。 加入20%NaOH水溶液(在2L水中1.2Kg NaOH)溶液,将pH调节至12,保持温度在0℃。用乙醚(3.x.250mL)萃取反应混合物,洗涤 用水,盐水洗干。 除去溶剂并通过分馏纯化,得到2-溴-4-甲基吡啶(164g,86%),为浅黄色液体。
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