化学合成。
医药合成中间体
合成路线 1（1. 合成：944401-56-3）
产率：94%
合成条件：With N-Bromosuccinimide In dichloromethane at 25℃; for 2 h; Darkness
实验步骤：向化合物28（500mg，3.1mmol）的DCM（40mL）溶液中加入NBS（600mg，3.3mmol）。 将溶液在室温下在室温下搅拌2小时。 然后用1N NaOH（50mL）淬灭反应，并用DCM（50mL）萃取。 将有机相用盐水（100mL）洗涤，用Na 2 SO 4干燥，过滤并浓缩。 将残余物用硅胶柱色谱法纯化，用石油醚：乙酸乙酯（10：1）洗脱，得到化合物29（700mg，94％），为浅黄色固体。 'H NIVIR（CDC13）：8.28（s，1H），6.77（s，1H），4.78（bs，2H）。
参考文献：
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合成路线 2
产率：96%
合成条件：With N-Bromosuccinimide In N,N-dimethyl-formamide at 5 - 20℃;
实验步骤：通用方法：19.1 5-溴-6-氯 - 吡啶-2-基胺将6-氯 - 吡啶-2-基胺（购自Aldrich）（1.50g，11.7mmol）溶于15ml N，N-二甲基甲酰胺中并冷却 加入1-溴 - 吡咯烷-2,5-二酮（2.28g，12.8mmol），将混合物缓慢升温至室温。 将混合物倒入冰水中，过滤收集沉淀物并真空干燥。 产率：理论质谱（ESI-）的91％：m / z = 207,209 [M + H] +
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