化学合成。
化学合成
合成路线 1(1. 合成:60956-25-4)
产率:37%
合成条件:at -10℃; for 1 h;
实验步骤:实施例58N4-(5-环丙基吡啶-1HH-吡咯烷酰基-33-yyll)) - NN22 - ((1-(5-甲基-1H-吲哚-1-基)甲基)嘧啶-2 4-二胺(1-122)步骤1:在-10℃下向2-溴-1,3-二甲基苯(5.0g,27.03mmol)在硫酸(98%,40mL)中的混合物中滴加 硝酸(68%,2.74g,27.03mmol)的硫酸(98%,10mL)溶液。反应完成后,将混合物在-10℃下搅拌1小时。将反应混合物倒入冰中 (200g)过滤得到的固体,用水洗涤,真空干燥。粗产物经SiO 2色谱纯化,用石油醚/ EtOAc(100:1)作为洗脱溶剂洗脱,得到2.3g(37%)2-溴。 -13,3-二甲基-4-硝基苯,为黄色固体(298):1U NMR(500MHz,DMSO-i):δ7.79(d,J = 8.5,1H),7.43(d,J = 8.5,1H) ),2.47(s,3H),2.44(s,3H)。
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