化学合成。
化学合成
合成路线 1(1. 合成:27561-51-9)
产率:94%
合成条件:With carbon tetrabromide; triphenylphosphine In dichloromethane at 20 - 25℃; for 2 h;
实验步骤:1-溴-4-(溴甲基)-2-甲基苯的制备向(4-溴-3-甲基苯基)甲醇(27.5g,136.8mmol)的二氯甲烷(250mL)溶液中加入PPh 3(39.4) g,150.5mmol)和CBr 4(49.9g,150.5mmol),将混合物在室温下搅拌2小时。 加入水。 分离有机层,用无水硫酸钠干燥并浓缩。 通过色谱法纯化粗产物,得到1-溴-4-(溴甲基)-2-甲基苯(34g,94%)。 1 H NMR(400MHz,CDCl 3)δ7.94-7.92(d,1H),7.70(s,1H),7.53-7.51(d,1H),4.86(s,2H),2.83(s,3H)。
参考文献:
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