4857-04-9 2-氯甲基苯并咪唑

危险性质：非危险化学品

化学合成，用于制造染料及颜料。

化学合成; 染料及颜料制造

合成路线 1（1. 合成：4857-04-9）

产率：93% 合成条件：With hydrogenchloride In waterReflux 实验步骤：通用方法：将适当的1,2-二氨基苯衍生物（0.1mol）和适当的羧酸衍生物（0.15mol）在100ml 5N HCl中的混合物加热至回流并搅拌3-5小时。 将反应混合物冷却至室温后，用碳酸氢钠中和。 通过抽滤过滤形成的沉淀，用水洗涤并干燥。 参考文献：

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合成路线 2（2. 合成：4857-04-9）

产率：91.3% 合成条件：With hydrogenchloride In water at 110℃; for 4 h; 实验步骤：将苯-1,2-二胺（2.0g，18.0mmol）和2-氯乙酸乙酯（2.6mL，24.0mmol）的混合物溶解在稀盐酸溶液（4mol / L，16mL）中。 将溶液在110℃加热4小时，然后冷却至室温。将反应溶液倒入冰水中，然后用氢氧化铵中和至pH9。 过滤沉淀物，用水洗涤，并在红外灯下干燥，得到化合物13f（2.7g，91.3％），为白色固体。 参考文献：

• [1] Molecules, 2017, vol. 22, # 11, [2] European Journal of Medicinal Chemistry, 2011, vol. 46, # 5, p. 1706 - 1712

合成路线 3（3. 合成：4857-04-9）

产率：82% 合成条件：With tin(ll) chloride In ethanol for 6 h; Reflux 实验步骤：2-（氯甲基）-1H-苯并[d]咪唑（3a-f）的合成与对化合物3a所述的相同。 在室温下，将SnCl 2（0.1mmol）加入搅拌的邻苯二胺（1,1mmol）和4-氯-3-氧代丁酸乙酯（2,1mmol）的EtOH（2mL）溶液中。将混合物在回流下搅拌 持续6小时 通过薄层色谱（TLC）监测反应完成后，在减压下除去溶剂。 将粗产物进行柱色谱（己烷= AcOEt 84:16），得到纯的苯并咪唑。 参考文献：

• [1] Green Chemistry, 2017, vol. 19, # 24, p. 5818 - 5830 [2] Synthetic Communications, 2015, vol. 45, # 14, p. 1642 - 1651