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    PROCESS FOR THE PREPARATION OF CYCLEN
    2.
    发明公开
    PROCESS FOR THE PREPARATION OF CYCLEN 审中-公开

    公开(公告)号：US20240190830A1

    公开(公告)日：2024-06-13

    申请号：US18284515

    申请日：2022-03-23

    Applicant: BRACCO IMAGING S.P.A. ,  SERICHIM SRL

    Inventor： Walter BARATTA ,  Rosario FIGLIOLIA ,  Pietro DELOGU ,  Ilaria ADAMO ,  Mariangela BOCCALON ,  Federica BUONSANTI

    IPC: C07D257/00

    CPC classification number: C07D257/00

    Abstract: The present invention relates to a process for the preparation of Cyclen. in its turn widely employed in the manufacturing of a variety of macrocyclic gadolinium complexes for use as MRI contrast agents. The said process comprises an efficient coupling of glyoxal with triethylene tetramine and the subsequent reduction of the obtained intermediate derivative with an aluminium based reducing agent. The process is particularly advantageous for the industrial scale as it avoids the use and/or formation of hazardous compounds and further provides for Cyclen manufacturing in high yields and purity.

    CONTINUOUS PROCESS FOR THE PREPARATION OF (S)-2-ACETYLOXYPROPIONIC ACID CHLORIDE
    5.
    发明申请
    CONTINUOUS PROCESS FOR THE PREPARATION OF (S)-2-ACETYLOXYPROPIONIC ACID CHLORIDE 有权
    制备（S）-2-乙酰氧基丙酸氯化物的连续方法

    公开(公告)号：US20150329464A1

    公开(公告)日：2015-11-19

    申请号：US14650868

    申请日：2013-12-04

    Applicant: BRACCO IMAGING S.P.A.

    Inventor： Silvia CERAGIOLI ,  Pietro DELOGU ,  Armando MORTILLARO ,  Alfonso NARDELLI ,  Stefano SGUASSERO ,  Rosario VELARDI ,  Carlo Felice VISCARDI

    IPC: C07C67/313 ,  C07C71/00

    CPC classification number: C07C67/313 ,  C07C67/08 ,  C07C67/287 ,  C07C71/00 ,  Y02P20/582 ,  C07C69/14

    Abstract: The present invention relates to a continuous method for the preparation of (S)-2-acetyloxypropionic acid from an aqueous solution of lactic acid and acetic anhydride, in acetic acid. (S)-2-acetyloxypropionic acid is used for the preparation of (S)-2-acetyloxypropionic acid chloride, an essential intermediate compound for the preparation of lopamidol and has to be industrially produced with high purity and suitable quality for producing lopamidol according to the Pharmacopoeia requirements. The continuous process according to the invention, comprises therefore also the chlorination steps of (S)-2-acetyloxypropionic acid with thionyl chloride to give the corresponding (S)-2-acetyloxypropionic acid chloride which is further distilled to give the suitable purity characteristics for its use for the preparation of non-ionic iodinated contrast agents as lopamidol.

    Abstract translation: 本发明涉及在乙酸中由乳酸和乙酸酐的水溶液制备（S）-2-乙酰氧基丙酸的连续方法。 （S）-2-乙酰氧基丙酸用于制备（S）-2-乙酰氧基丙酸氯化物，其是制备洛帕糖醇的必需中间体化合物，并且必须在工业上以高纯度生产，并且根据 药典要求。 根据本发明的连续方法还包括（S）-2-乙酰氧基丙酸与亚硫酰氯的氯化步骤，得到相应的（S）-2-乙酰氧基丙酰氯，进一步蒸馏得到适合的纯度特性， 其用于制备非离子碘化造影剂作为洛帕糖醇。

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