1131-40-4 1-溴-2,4,6-三甲氧基苯

合成路线 3（3. 合成：1131-40-4）

产率：98% 合成条件：With N-Bromosuccinimide In neat (no solvent) at 20℃; for 0.75 h; Milling; Green chemistry 实验步骤：一般步骤：将1-甲氧基-3,5-二甲基苯（100mg，0.73mmol），N-溴代琥珀酰亚胺（NBS，260mg，1.46mmol）和一个球（5mm直径，不锈钢）转移到研磨罐中（10mL） ， 不锈钢）。进行球磨操作，通过TLC / 1H NMR监测反应进程。[1]完成后，将反应混合物转移到30mL乙酸乙酯中并在0℃冷却。在纸过滤时将产物分离为滤液，并将废琥珀酰亚胺作为沉淀物分离。将所得滤液真空浓缩，分离出250mg（产率：85％）2b，为无色粉末。为了大规模测试效率，还进行了以1.3g规模对1-甲氧基-3,5-二甲基苯进行单溴化反应1小时的反应，并且以87％的收率分离产物[1]。停止研磨设备并从反应罐中收集小部分样品以研究TLC /质子NMR。接着，再次开始反应，排除该操作时间以报告反应时间。 参考文献：

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