化学合成。
化学合成
合成路线 1(1. 合成:103347-14-4)
产率:100%
合成条件:With N-Bromosuccinimide; dibenzoyl peroxide In tetrachloromethane for 1 h; Reflux
实验步骤:向CCl(2.5L)中的2-氯-5-甲基苯甲醚(11)(274g,1.75mol)溶液中加入过氧化苯甲酰(4.23g,0.02mol)和NBS(321g,1.80mol)。 在机械搅拌下将反应混合物加热至回流1小时。 冷却反应混合物,用1N HCl(2L),饱和NaHCO 3(2L)和盐水(2L)洗涤,经MgSO 4干燥,过滤并减压浓缩,得到5-(溴甲基)-3-氯苯甲醚。 (12)为淡黄色固体(412g,定量)。 1 H NMR(400MHz,CDCl 3):δ7.30-7.34(d,1H),6.95(s,1H),6.91-6.93(d,1H),4.45(s,2H),3.92(s,3H)。
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