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    SEMI-SYNTHESIS PROCEDURES
    2.
    发明申请
    SEMI-SYNTHESIS PROCEDURES 审中-公开

    公开(公告)号：US20190210988A1

    公开(公告)日：2019-07-11

    申请号：US16059857

    申请日：2018-08-09

    申请人： Tetraphase Pharmaceuticals, Inc.

    发明人： Wu-Yan Zhang ,  Danny LaFrance ,  Magnus P. Ronn

    IPC分类号： C07D295/15 ,  C07C237/26 ,  C07C245/20 ,  C07C231/12 ,  C07D207/06

    CPC分类号： C07D295/15 ,  C07C231/12 ,  C07C237/26 ,  C07C245/20 ,  C07C2603/46 ,  C07D207/06

    摘要： Provided herein are improved processes for converting C7-amino-substituted tetracyclines to C7-fluoro-substituted tetracyclines, as well as intermediates produced by or used in these processes. In one embodiment, a thermal fluorination method is provided in which a suspension comprising a non-polar organic solvent and a C7-diazo-substituted tetracycline hexafluorophosphate, hexafluoroarsenate or hexafluorosilicate salt, or a salt, solvate or combination thereof, is heated to provide a C7-fluoro-substituted tetracycline, or salt, solvate or combination thereof. In another embodiment, a photolytic fluorination is provided in which a solution comprising an ionic liquid and a C7-diazo-substituted tetracycline tetrafluoroborate, hexafluorophosphate, hexafluoroarsenate or hexafluorosilicate salt, or a salt, solvate or combination thereof, is irradiated to provide a C7-fluoro-substituted tetracycline, or salt, solvate or combination thereof.

    Crystalline minocycline base and processes for its preparation
    7.
    发明授权
    Crystalline minocycline base and processes for its preparation 有权
    结晶米诺环素碱及其制备方法

    公开(公告)号：US09416097B2

    公开(公告)日：2016-08-16

    申请号：US13599116

    申请日：2012-08-30

    申请人： Zita Mendes ,  Jose Rafael Antunes ,  Susana Marto ,  William Heggie

    发明人： Zita Mendes ,  Jose Rafael Antunes ,  Susana Marto ,  William Heggie

    IPC分类号： C07C237/26

    CPC分类号： C07C237/26

    摘要： The invention provides crystalline minocycline base. In particular, three crystalline polymorphic forms, designated Form I, Form II and Form III, of minocycline base are provided. These are characterized by XRD and IR data. Processes for preparing the new polymorphic forms are also provided. For example, Form I is prepared by dissolving and/or suspending amorphous minocycline base in an organic solvent chosen from ethers followed by crystallization from the mixture.

    摘要翻译： 本发明提供了结晶米诺环素碱。 特别地，提供了三环结构的多晶型形式，称为米诺环素碱的I型，II型和III型。 其特征在于XRD和IR数据。 还提供了制备新多晶型体的方法。 例如，通过将无定形米诺环素碱溶解和/或悬浮在选自醚中的有机溶剂中，然后从混合物中结晶来制备形式I。