化学合成。
化学合成
合成路线 1(1. 合成:63286-28-2)
产率:96%
合成条件:With hydrazine hydrate In ethanol; waterReflux
实验步骤:步骤1:向2,3-二氯吡嗪(150g,1.00mol)的EtOH(700mL)溶液中加入一水合肼(124.53g,2.11mmol,85%水溶液)。 将反应混合物在回流下加热过夜。 冷却反应混合物并过滤沉淀物。 将所得固体用水(100mL,两次)洗涤,然后用冷EtOH(150ml,两次)洗涤,并在减压下干燥,得到2-氯-3-肼基吡嗪(140g,产率96%)。
参考文献:
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合成路线 2(2. 合成:63286-28-2)
产率:73%
合成条件:With hydrazine In ethanol; water
实验步骤:将2,3-二氯吡嗪(2mL,13mmol)溶于95%乙醇(4mL)中,在搅拌下向其中滴加无水肼(2mL,67mmol)。 在加入肼的过程中,溶液变热并变黄。 在冰浴中冷却该混合物后,通过过滤分离所得物质,用冷的95%乙醇水溶液洗涤,得到1-(3-氯吡嗪-2-基)肼(1.42g,73%收率),为白色晶体。 没有进一步纯化。 MS m / z:145.0(M + 1)。
参考文献:
- [1] Patent: WO2009/64418, 2009, A1. Location in patent: Page/Page column 85