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    • 16. 发明授权
    • Preparation of bis-(1(2)H-tetrazol-5-yl)-amine monohydrate
    • 制备双 - (1(2)H-四唑-5-基) - 胺一水合物
    • US06570022B2
    • 2003-05-27
    • US09957938
    • 2001-09-21
    • Darren L. NaudMichael A. Hiskey
    • Darren L. NaudMichael A. Hiskey
    • C07D40312
    • C07D257/06
    • A process of preparing bis-(1(2)H-tetrazol-5-yl)-amine monohydrate is provided including combining a dicyanamide salt, an azide salt and water to form a first reaction mixture, adding a solution of a first strong acid characterized as having a pKa of less than about 1 to said first reaction mixture over a period of time characterized as providing a controlled reaction rate so as to gradually form hydrazoic acid without loss of significant quantities of hydrazoic acid from the solution while heating the first reaction mixture at temperatures greater than about 65° C., heating the resultant reaction mixture at temperatures greater than about 65° C. for a period of time sufficient to substantially completely form a reaction product, treating the reaction product with a solution of a second strong acid to form a product of bis-(1(2)H-tetrazol-5-yl)-amine monohydrate, and, recovering the bis-(1(2)H-tetrazol-5-yl)-amine monohydrate product.
    • 提供制备双 - (1(2)H-四唑-5-基) - 胺一水合物的方法,包括将二氰胺盐,叠氮盐和水混合以形成第一反应混合物,加入第一强酸 其特征在于在一段时间内具有小于约1的所述第一反应混合物的pKa,其特征在于提供受控的反应速率,以便在加热第一反应的同时逐渐形成叠氮酸,而不会从溶液中流失显着量的叠氮酸 混合物,在大于约65℃的温度下,将所得反应混合物在大于约65℃的温度下加热足以基本上完​​全形成反应产物的时间,用第二个强力的溶液处理反应产物 酸形成双 - (1(2)H-四唑-5-基) - 胺一水合物的产物,并回收双 - (1(2)H-四唑-5-基) - 胺一水合物产物。