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    • 28. 发明授权
    • 4-azido-4,4-dinitro-1-butanol and derivatives thereof
    • 4-叠氮基-4,4-二硝基-1-丁醇及其衍生物
    • US4795593A
    • 1989-01-03
    • US82775
    • 1987-08-05
    • Milton B. FrankelJames F. Weber
    • Milton B. FrankelJames F. Weber
    • C06B25/00C07C205/15C07C117/00
    • C07C205/15C06B25/00C07C205/44C07C247/00
    • There is provided the compound 4-azido-4,4-dinitro-1-butanol (ADNBOH) and a method for making same which comprises reacting trinitromethane and acrolein at a reduced temperature to provide 4,4,4-trinitro-butyraldehyde (TNBAl), reducing the TNBSl to provide 4,4-trinitro-1-butanol (TNBOH) which is further reduced to provide 4,4-dinitro-1-butanol (DNBOH), reacting the DNBOH with acetyl chloride to provide 4,4-dinitro-1-butyl acetate (DNBAc), reacting the DNBAc with an alkali metal azide in an electrolysis cell to provide 4-azido-4,4-dinitro-1-butyl acetate (ADNBAc) and reacting the ADNBAc with a lower alcohol and recovering the 4-azido-4,4-dinitro-1-butanol (ADNBOH).Also provided are several azidodinitro derivatives of 4-azido-4,4-dinitro-1-butanol and methods for making same.
    • 提供化合物4-叠氮基-4,4-二硝基-1-丁醇(ADNBOH)及其制备方法,其包括在降低的温度下使三硝基甲烷和丙烯醛反应,得到4,4,4-三硝基丁醛(TNBAl ),还原TNBS1以提供4 - 三硝基-1-丁醇(TNBOH),进一步还原以提供4,4-二硝基-1-丁醇(DNBOH),使DNBOH与乙酰氯反应,得到4,4-二硝基-1-丁醇 二丁基-1-丁基乙酸酯(DNBAc),使DNBAc与电解槽中的碱金属叠氮化物反应,得到4-叠氮基-4,4-二硝基-1-丁酸乙酯(ADNBAc),并使ADNBAc与低级醇和 回收4-叠氮基-4,4-二硝基-1-丁醇(ADNBOH)。 还提供了4-叠氮基-4,4-二硝基-1-丁醇的几种叠氮基硝基衍生物及其制备方法。
    • 29. 发明授权
    • Process for preparing 1,5-diazido-3-nitrazapentane
    • 制备1,5-二叠氮基-3-硝基氮烷的方法
    • US4761250A
    • 1988-08-02
    • US764048
    • 1985-08-09
    • Milton B. FrankelEdward F. Witucki
    • Milton B. FrankelEdward F. Witucki
    • C07C247/04C06B25/34C07C67/00C07C241/00C07C117/00
    • C07C247/00
    • A process for producing 1,5-diazido-3-nitrazapentane (DANPE) which comprises the steps of nitrating diethanolamine with nitric acid in a halogenated solvent such as methylene chloride to form 1,5-dinitrato-3-nitrazapentane (DINA) as intermediate, solvent transferring such intermediate from the halogenated solvent to dimethylsulfoxide, adding sodium azide to the resulting solution to form DANPE as product, and solvent transferring such product from the dimethylsulfoxide to another halogenated solvent, e.g. methylene chloride. Thus, both DINA intermediate and DANPE product are prepared in solution, and both can also be purified in solution, eliminating the necessity for isolating the neat, hazardous compounds. The DANPE product can be further solvent transferred from the halogenated solvent to ethyl acetate to form an ethyl acetate solution of DANPE, which can be used to furnish the DANPE as an energetic plasticizer, e.g. in the production of gun propellants.
    • 一种制备1,5-二叠氮基-3-硝基氮烷(DANPE)的方法,其包括在卤化溶剂如二氯甲烷中用硝酸硝化二乙醇胺以形成中间体1,5-二硝基-3-硝基氮烷(DINA) 将这样的中间体从卤代溶剂转移到二甲基亚砜中,向所得溶液中加入叠氮化钠以形成DANPE作为产物,以及将这种产物从二甲基亚砜转移到另一种卤化溶剂中的溶剂,例如 二氯甲烷。 因此,在溶液中制备了DINA中间体和DANPE产品,并且两者都可以在溶液中纯化,从而无需分离纯净的有害化合物。 DANPE产物可以进一步从卤化溶剂转移到乙酸乙酯中以形成DANPE的乙酸乙酯溶液,其可用于提供DANPE作为能量增塑剂,例如, 在枪式推进剂的生产中。