Method for preparing clopidogrel 1,5-naphthalenedisulfonate or hydrate thereof
    12.
    发明授权
    Method for preparing clopidogrel 1,5-naphthalenedisulfonate or hydrate thereof 失效
    制备1,5-萘二磺酸氯吡格雷或其水合物的方法

    公开(公告)号:US07612207B2

    公开(公告)日:2009-11-03

    申请号:US12293959

    申请日:2007-03-16

    CPC classification number: C07D495/04

    Abstract: The present invention relates to a method for preparing clopidogrel 1,5-naphthalenedisulfonate or a hydrate thereof, which comprises reacting a clopidogrel-acid addition salt with disodium 1,5-naphthalenedisulfonate or its hydrate in water, or a mixture of water and an organic solvent. High quality clopidogrel 1,5-naphthalenedisulfonate can be prepared by the inventive method by way of using non-corrosive disodium 1,5-naphthalenedisulfonate.

    Abstract translation: 本发明涉及一种氯吡格雷1,5-萘二磺酸盐或其水合物的制备方法,该方法包括使氯吡格雷酸加成盐与1,5-萘二磺酸二钠或其水合物在水中或水与有机物的混合物 溶剂。 通过本发明方法可以通过使用1,5-萘二磺酸非腐蚀性二钠制备高质量的氯萘吡格雷1,5-萘二磺酸盐。

    Method of preparing form II crystals of clarithromycin
    20.
    发明授权
    Method of preparing form II crystals of clarithromycin 失效
    制备克拉霉素II型晶体的方法

    公开(公告)号:US06515116B2

    公开(公告)日:2003-02-04

    申请号:US09805831

    申请日:2001-03-14

    CPC classification number: C07H17/08 Y02P20/55

    Abstract: High purity Form II crystals of clarithromycin can be easily prepared in a high yield by a process comprising the steps of: protecting the 9-oxime hydroxy group of erythromycin A 9-oxime or a salt thereof with a tropyl group and the 2′- and 4″-hydroxy groups with trimethylsilyl groups; reacting 2′,4″-O-bis(trimethylsilyl)erythromycin A 9-O-tropyloxime with a methylating agent; removing the protecting groups and the oxime group of 2′,4″-O-bis(trimethylsilyl)-6-O-methylerythromycin A 9-O-tropyloxime to obtain crude clarithromycin; treating the crude clarithromycin with methanesulfonic acid in a mixture of a water-miscible organic solvent and water to obtain crystalline clarithromycin mesylate trihydrate; and neutralizing the crystalline clarithromycin mesylate trihydrate with aqueous ammonia in a mixture of a water-miscible organic solvent and water.

    Abstract translation: 克拉霉素的高纯度II型晶体可以通过包括以下步骤的方法以高产率容易地制备:保护红霉素A 9-肟的9-肟羟基或其盐与丙基和2'-和 4“ - 羟基与三甲基甲硅烷基; 使2',4“ - O-双(三甲基甲硅烷基)红霉素A 9-O-草丙基肟与甲基化试剂反应; 除去2',4“-O-双(三甲基甲硅烷基)-6-O-甲基红霉素A 9-O-草丙基肟的保护基和肟基,得到粗克拉霉素; 在水混溶性有机溶剂和水的混合物中用甲磺酸处理粗克拉霉素,得到结晶克拉硫霉素甲磺酸盐三水合物; 并用水混溶性有机溶剂和水的混合物用氨水中和结晶克拉硫酸甲磺酸盐三水合物。

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