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    Synthesis of bis(thio-hydrazide amide) salts
    81.
    发明申请
    Synthesis of bis(thio-hydrazide amide) salts 失效
    双（硫代酰肼）酰胺盐的合成

    公开(公告)号：US20060270873A1

    公开(公告)日：2006-11-30

    申请号：US11432307

    申请日：2006-05-11

    申请人： Shoujun Chen ,  Zhi-Qiang Xia

    发明人： Shoujun Chen ,  Zhi-Qiang Xia

    IPC分类号： C07C327/40

    CPC分类号： C07C327/56 ,  C07C2601/02 ,  C07C2601/04 ,  C07C2601/08 ,  C07C2601/14

    摘要： A method of preparing a bis(thio-hydrazide amide) disalt includes the steps of combining a neutral bis(thio-hydrazide amide), an organic solvent and a base to form a bis(thio-hydrazide amide) solution; and combining the solution and methyl tert-butyl ether, thereby precipitating a disalt of the bis(thio-hydrazide amide). In some embodiments, a method of preparing a bis(thio-hydrazide amide) disalt includes the steps of combining a neutral bis(thio-hydrazide amide) and an organic solvent selected from methanol, ethanol, acetone, and methyl ethyl ketone to make a mixture; adding at least two equivalents of a base selected from sodium hydroxide, potassium hydroxide, sodium methoxide, potassium methoxide, sodium ethoxide and potassium ethoxide to the mixture, thereby forming a solution; and combining the solution and methyl tert-butyl ether to precipitate the disalt of the bis(thio-hydrazide amide). The disclosed methods do not require lyophylization and the solvents used in the process can be more readily removed to low levels consistent with pharmaceutically acceptable preparation.

    摘要翻译： 制备双（硫代 - 酰肼酰胺）二盐的方法包括将中性双（硫代酰肼）酰胺，有机溶剂和碱组合以形成双（硫代 - 酰肼酰胺）溶液的步骤; 并将该溶液与甲基叔丁基醚混合，从而沉淀出双（硫代 - 酰肼）酰胺的混合物。 在一些实施方案中，制备双（硫代 - 酰肼酰胺）二盐的方法包括将中性双（硫代酰肼）酰胺和选自甲醇，乙醇，丙酮和甲基乙基酮的有机溶剂合并以制备 混合物; 向混合物中加入至少两当量的选自氢氧化钠，氢氧化钾，甲醇钠，甲醇钾，乙醇钠和乙醇钾的碱，从而形成溶液; 并将该溶液和甲基叔丁基醚混合以沉淀双（硫代 - 酰肼）酰胺的混合物。 所公开的方法不需要冻干，并且可以更容易地将该方法中使用的溶剂除去至与药学上可接受的制剂一致的低水平。