-
公开(公告)号：US20040132996A1
公开(公告)日：2004-07-08
申请号：US10694619
申请日：2003-10-27
申请人： LUPIN LIMITED
IPC分类号： C07D501/14
CPC分类号： C07D501/00
摘要： A process for preparation of ceftiofur sodium of formula (Ib) 1 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) 2 nullwherein 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 null5null C. to 30null C. to give after necessary neutralisation 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; 3 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 null10null C. to 10null 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）使用摩尔比为1.5至3.0的头孢噻肟或其盐或其通式（VI）的酯，其中R 3为氢，碱金属或碱土金属或易水解的酯与硫代呋喃酸反应 摩尔每摩尔化合物（Ⅵ）在乙腈作为溶剂存在下和在大量过量的甲磺酸存在下，以摩尔比例为12至18摩尔/摩尔化合物（Ⅵ），并且在 在-5℃至30℃下，在必要时中和碱金属或碱土金属或除去适用的具有高稳定性的式（Ia）头孢噻呋酯的4-羧酸官能团的酯基， 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）将由此获得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反应并在亚硫酸氢钠的存在下反应，得到式（Ib）的头孢噻肟钠，
搜索结果
1 条记录 (耗时 0.023 秒)
