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    Method for manufacture of ceftiofur
    6.
    发明授权
    Method for manufacture of ceftiofur 失效
    头孢噻呋的制造方法

    公开(公告)号：US07511135B2

    公开(公告)日：2009-03-31

    申请号：US10532194

    申请日：2003-10-27

    申请人： Om Dutt Tyagi ,  Santosh Kumar Richhariya ,  Rajesh Kumar Ramchandra Pawar ,  Yuvaraj Atmaram Chavan

    发明人： Om Dutt Tyagi ,  Santosh Kumar Richhariya ,  Rajesh Kumar Ramchandra Pawar ,  Yuvaraj Atmaram Chavan

    IPC分类号： C07D501/36

    CPC分类号： C07D417/14

    摘要： A process for preparation of ceftiofur of formula (I) having purity greater than 97% is disclosed. The process comprises reacting [2-(2-aminothiazol-4-yl)]-2-syn-methoxyimino acetic acid-2-benzothiazolyl thioester of formula (II), with 7-amino-3-(2-furanylcarbonylthiomethyl)-3-cephem-4-carboxylic acid of formula (III) in the presence of a mixture of an water-immiscible inert organic solvent and water and in the presence of a organic base and isolating ceftiofur of formula (I) substantially free of impurities by, a) adding water to the reaction mixture and selectively partitioning the impurities in the organic phase and ceftiofur (I) in the form of a salt with the base in the aqueous phase, b) acidifying the aqueous phase containing ceftiofur (I) in the form of a salt with the base in the presence of a mixture containing a water-miscible and a water-immiscible organic solvent and in the presence of a saturated aqueous solution of an alkali or alkaline earth containing salt, to partition ceftiofur (I) in the organic phase, and c) isolating ceftiofur (I) of high purity and substantially free of impurities by evaporation of the organic solvent or precipitation by addition of a anti-solvent.

    摘要翻译： 公开了制备具有大于97％纯度的式（I）头孢噻呋的方法。 该方法包括使式（II）的[2-（2-氨基噻唑-4-基）] - 2-顺式 - 甲氧基亚氨基乙酸-2-苯并噻唑基硫代酯与7-氨基-3-（2-呋喃基羰硫基甲基）-3 （III）的头孢-4-羧酸在水不混溶的惰性有机溶剂和水的混合物存在下，在有机碱的存在下，分离式（I）的头孢噻呋基本上不含杂质， a）向反应混合物中加入水，并在水相中选择性地分配有机相中的杂质和与碱的盐形式的头孢噻呋（I），b）以含有头孢噻呋（I）的形式酸化含有头孢噻呋 在含有水混溶性和与水不混溶的有机溶剂的混合物存在下，在含有碱或碱土金属盐的饱和水溶液的存在下，将碱与碱反应，从而将头孢噻吩（I） 有机相，和c）分离高纯度和实质的头孢噻呋（I） 通过蒸发有机溶剂或通过加入抗溶剂沉淀而不含杂质。

    Method for preparation of ceftiofur and salts thereof
    8.
    发明授权
    Method for preparation of ceftiofur and salts thereof 失效
    头孢噻呋及其盐的制备方法

    公开(公告)号：US07335767B2

    公开(公告)日：2008-02-26

    申请号：US10694619

    申请日：2003-10-27

    申请人： Om Dutt Tyagi ,  Santosh Kumar Richhariya ,  Rajesh Kumar Ramchandra Pawar

    发明人： Om Dutt Tyagi ,  Santosh Kumar Richhariya ,  Rajesh Kumar Ramchandra Pawar

    IPC分类号： C07D501/36

    CPC分类号： C07D501/00

    摘要： A process for preparation of ceftiofur sodium of formula (Ib) possessing high stability and having purity of more than 97% and substantially free of impurities, is disclosed. The process comprises: i) reacting cefotaxime or its salts or its esters of formula (VI) wherein R3 is hydrogen, an alkali or alkaline earth metal, or an easily hydrolysable ester, with thiofuroic acid, employed in a molar proportion of 1.5 to 3.0 moles per mole of compound (VI), in the presence of acetonitrile as solvent and in the presence of large excess of methanesulfonic acid, employed in molar proportions of 12 to 18 moles per mole of compound (VI), and at a temperature of between −5° C. to 30° C. to give after necessary neutralization of the alkali or alkaline earth metal or removal of the ester group of the 4-carboxylic acid function, wherever applicable, ceftiofur of formula (Ia), possessing high stability and having purity of more than 97% and substantially free of impurities; ii) converting the ceftiofur of formula (Ia) thus obtained to its salt with an organic amine by treating a solution of ceftiofur in a mixture of water and a water-miscible organic solvent with an organic amine, at a temperature ranging from −10° C. to 10° C.; iii) reacting of the amine salt thus obtained with a sodium metal carrier in a mixture of water and water-miscible organic solvent and in presence of sodium hydrogen sulfite to give ceftiofur sodium of formula (Ib).

    摘要翻译： 公开了制备具有高稳定性和纯度大于97％且基本上不含杂质的式（Ib）头孢噻呋钠的方法。 该方法包括：i）将头孢噻肟或其盐或其其中R 3为氢的式（VI）的酯，碱金属或碱土金属或易水解的酯与硫代呋喃酸反应， 摩尔比例为1.5-3.0摩尔/摩尔化合物（Ⅵ），在乙腈作为溶剂的存在下，在大量过量的甲磺酸的存在下，摩尔比例为12至18摩尔/摩尔化合物（Ⅵ ），并且在-5℃至30℃的温度下进行，必要时中和碱金属或碱土金属或除去4-羧酸官能团的酯基（如果适用的话），式 （Ia），具有高稳定性，纯度大于97％，基本上不含杂质; ii）通过在-10℃的温度范围内用有机胺处理水与水混溶性有机溶剂的混合物中的头孢噻肟溶液，将有机胺衍生的式（Ia）头孢噻吩转化为其盐 ℃至10℃。 iii）将由此得到的胺盐与水和水混溶性有机溶剂的混合物中的钠金属载体与亚硫酸氢钠的混合物反应，得到式（Ib）的头孢噻肟钠。