化学合成。
医药; 农药; 合成香料
合成路线 1(1. 合成:2859-78-1)
产率:91%
合成条件:With dihydrogen peroxide; ammonium bromide; acetic acid In water at 20℃; for 20 h;
实验步骤:实施例1:由藜芦醚制备4-溴-1,2-二甲氧基苯(1)向3.0L反应器中加入藜芦醚(142g,1.03mol)和溴化铵(110g,1.12mol,1.10当量)的乙酸溶液(1.6)L)。 将过氧化氢水溶液(30%)(180mL,1.76mol,1.67当量)滴加到反应混合物中,并将内容物在室温下搅拌。 20小时后,将反应混合物用饱和碳酸氢钠溶液处理,并用二氯甲烷(3×200mL)萃取。 将合并的有机萃取液用水(2×200mL)和盐水(200mL)洗涤,用无水硫酸钠干燥,然后减压蒸发,得到黄色液体。 蒸馏后,得到纯产物(202.7g,沸点128-133℃/ 10毫巴,91%)。 3 / 4NMR(400MHz,DMSO-13C NMR(100MHz,DMSO-“3/4):δ150.3,148.8,123.5,115.3,113.8,112.3,56.2,56.0。
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