化学合成。
化学合成
合成路线 1(1. 合成:123148-78-7)
产率:100%
合成条件:With N-iodo-succinimide; sodium sulfate In ethanol; N,N-dimethyl-formamide
实验步骤:步骤1. 4-氯-5-碘-7H-吡咯并[2,3-d]嘧啶(化合物3)4-氯-7H-吡咯并[2,3-d]嘧啶10.75g(70mmol)(Toronto Research 将化学品(Inc)和N-碘代琥珀酰亚胺(16.8g,75mmol)溶解在400mL无水DMF中,并在环境温度下在黑暗中放置过夜。 蒸发溶剂。 将黄色残余物悬浮在热的10%Na 2 SO 3溶液中,过滤,用热水洗涤两次并从乙醇中结晶,得到14.6g(74.6%)标题化合物,为灰白色晶体。 将母液蒸发至1/3体积并再次从乙醇中结晶,得到2.47g(12.3%)标题产物。 总收益率接近100%。
参考文献:
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合成路线 2(2. 合成:123148-78-7)
产率:86.9%
合成条件:at 20℃;
实验步骤:步骤1:将4-氯-7H-吡咯并[2,3-d]嘧啶10.75g(70mmol)和N-碘代琥珀酰亚胺(16.8g,75mmol)溶于400mL无水DMF中,并在环境温度下保持在室温下。 黑夜过夜。 蒸发溶剂。 将黄色残余物悬浮在热的10%Na 2 SO 3溶液中,过滤,用热水洗涤两次并从乙醇中结晶,得到14.6g(74.6%)标题化合物,为灰白色晶体。 将母液蒸发至体积并再次从乙醇中结晶,得到2.47g(12.3%)目标化合物。 总产率接近100%; Tm 212-214℃(dec);UVλmax:307,266,230,227nm(甲醇); MS:277.93(MH),313(M + Cl); 1H- NMR(DMSO-d6):12.94(s,1H,NH),8.58(s,1H),7.94(s,1H)。
参考文献:
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