化学合成。
化学合成
合成路线 1(1. 合成:99368-68-0)
产率:92%
合成条件:With iron; ammonium chloride In ethanol; water at 80℃; for 4 h;
实验步骤:向2-氯-5-硝基-3-(三氟甲基)吡啶(10.0g,44.1mmol)的乙醇:水溶液中加入:TH F锡(2:2:1,150mL),NH 4 Cl(16.53g) ,309mmol)和铁粉(17.26g,309mmol)。 将所得反应混合物在80℃下搅拌4小时。 反应完成后,将反应混合物冷却至室温,用硅藻土床过滤,滤液床用乙酸乙酯(200mL)洗涤。 浓缩合并的滤液,得到8.0g(92%)标题产物,为棕色固体。 1HNMR(400MHz,DMSO-d6)U7.93(d,J = 2.7Hz,1H),7.39(d,J = 2.8Hz,1H),6.02(s,2H); ESI-MS(m / z)197.26(MH)+。
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