化学合成。
有机原料
合成路线 1(1. 合成:608-72-0)
产率:80%
合成条件:With N-Bromosuccinimide In neat (no solvent) at 20℃; for 2 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。
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