作为中间体或原料用于医药、农药相关合成反应。
医药; 农药
合成路线 1(1. 合成:57559-52-1)
产率:59%
合成条件:With N-Bromosuccinimide; 2,2'-azobis(isobutyronitrile) In tetrachloromethane at 85℃; for 20 h;
实验步骤:中间体1:1-(溴甲基-4-甲氧基-2-硝基苯;向4-甲基-3-硝基苯甲醚(16.53mL; 119.64mmol; 1当量)的溶液中,在CCU(500mL)中加入N-溴代琥珀酰亚胺(21.29)。 g; 119.64mmol; 1eq)和偶氮二异丁腈(392.9mg; 2.39mmol; 0.02当量)。将混合物在85℃加热20小时。将溶液冷却至室温,过滤除去琥珀酰亚胺沉淀。 浓缩滤液,得到黄色油状物,油状物在-25℃下结晶一夜后,再溶于EtOAc(15mL)中,加入石油醚,在-25℃下2h后,化合物重结晶。 用石油醚洗涤,在真空下干燥固体,得到17.4g(59%)标题化合物,为液体.1H NMR(DMSO-dd)δ7.68(d,J = 8Hz,1H),7.56(d ,J = 3Hz,1H),7.33(dd,J = 8.0,3.0Hz,1H),4.89(s,2H),3.87(s,3H).HPLC(max plot)99%; Rt 4.09min。
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