化学合成。
化学合成
合成路线 1(1. 合成:880870-13-3)
产率:45%
合成条件:at 0 - 55℃; for 3 h;
实验步骤:将2-氯-4-甲氧基吡啶(13.3g,92.6mmol)溶于浓硫酸(65ml)中,在冰冷却下加入N-溴代琥珀酰亚胺(16.5g,92.6mmol),并在0℃下加热搅拌混合物。 55℃,3小时。 将反应混合物倒入冰水中,用8N氢氧化钠水溶液碱化,并用氯仿萃取。 用饱和盐水洗涤有机层,并用硫酸钠干燥。 过滤后,将滤液减压浓缩,并将残余物通过硅胶色谱法(己烷:乙酸乙酯= 9:1至5:1)纯化,得到目标产物,为白色固体(9.3g,收率45%)。 1H NMR(CDCl3 300MHz)(δ)ppm:3.97(3H,s),6.84(1H,s),8.34(1H,s)
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