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    • 5. 发明申请
    • Method for producing triazolinthion derivatives
    • 三唑衍生物的制备方法
    • US20020026058A1
    • 2002-02-28
    • US09795062
    • 2001-02-26
    • Manfred JautelatAchim HuppertsReinhard Lantzsch
    • C07D249/08
    • C07D249/12C07C337/06
    • According to a novel process, it is possible to prepare triazolinethione derivatives of the formula 1 in which R1 and R2 are each as defined in the description by a) reacting hydrazine derivatives of the formula 2 nullor their acid addition salts with an inorganic or organic acid with thiocyanate of the formula 3 nullin which Y represents sodium, potassium or ammonium nullin the presence of a diluent and, if appropriate, in the presence of a catalyst and b) reacting the resulting thiosemicarbazide derivatives of the formula 4 nullwith formic acid, if appropriate in the presence of a catalyst and if appropriate in the presence of a diluent. The thiosemicarbazide derivatives of the formula (IV) are novel.
    • 根据新的方法,可以制备下式的三唑啉硫酮衍生物,其中R1和R2各自如说明书中所定义:a)使下式的肼衍生物或其酸加成盐与无机或有机酸与硫氰酸酯反应 其中Y表示钠,钾或铵,在稀释剂存在下,如果合适的话,在催化剂存在下,和b)使所得到的硫代氨基脲衍生物与甲酸反应,如果合适的话,在 催化剂和如果合适的话,在稀释剂存在下。 式(IV)的硫代氨基脲衍生物是新颖的。
    • 8. 发明授权
    • Production of thiocarbohydrazide on a commercial scale
    • 以商业规模生产硫代碳酰肼
    • US4294985A
    • 1981-10-13
    • US48856
    • 1979-06-15
    • Gunther CrammKarl H. Blocher
    • Gunther CrammKarl H. Blocher
    • C07C327/56C01B20060101C07C20060101C07C67/00C07C325/00C07C335/40C07C337/06C07C159/00
    • C07C337/06
    • In the production of thiocarbohydrazide by reacting hydrazine hydrate with carbon disulphide in the presence of water to form in a first stage hydrazinium dithiocarbazinate, subsequently thermally decomposing the hydrazinium dithiocarbazinate in a second stage to form thiocarbohydrazide, and recovering the thiocarbohydrazide from the reaction medium, the improvement which comprises effecting the entire reaction in the mother liquor of a preceding batch, carrying out the first reaction stage at a temperature between about 25.degree. C. and 45.degree. C., with injection of carbon disulphide below the surface of the reaction mixture; carrying out the second stage at about 62.degree. to 65.degree. C. without prior isolation of the intermediate product; filtering off the thiocarbohydrazide formed after cooling, separating the amount of mother liquor in excess of that required for the next batch, and feeding the balance of the mother liquor to the next batch. The excess mother liquor not required for the next batch is heated to about 70.degree. to 75.degree. C., and after separating off the thiocarbohydrazide, the remaining mother liquor is subjected to combustion.
    • 在硫代碳酰肼的制备中,通过在水存在下使水合肼与二硫化碳反应,在第一阶段中形成二硫代肼基肼,然后在第二阶段热分解二硫代肼基肼,形成硫代碳酰肼,并从反应介质中回收硫代碳酰肼, 其包括进行前一批次的母液中的整个反应,在约25℃至45℃的温度下进行第一反应阶段,在反应混合物的表面下注入二硫化碳; 在大约62°至65℃进行第二阶段,而不预先分离中间产物; 过滤冷却后形成的硫代碳酰肼,将母液的量分离超过下一批所需的母液量,并将母液的余量送入下一批。 将下一批不需要的过量母液加热至约70℃至75℃,分离硫代碳酰肼后,将剩余的母液进行燃烧。