CN110198931A - 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的制备方法 - Google Patents

1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的制备方法 Download PDF

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Publication number
CN110198931A
CN110198931A CN201780080570.8A CN201780080570A CN110198931A CN 110198931 A CN110198931 A CN 110198931A CN 201780080570 A CN201780080570 A CN 201780080570A CN 110198931 A CN110198931 A CN 110198931A
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water
added
cyclen
acid
reaction
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CN110198931B (zh
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孟周钧
魏彦君
邢艳平
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Weizhi Pharmaceutical Co ltd
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Viwit Pharmaceutical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D257/00—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms
    • C07D257/02—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms not condensed with other rings

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

本发明公开了一种1,4,7,10‑四氮杂环十二垸‑1,4,7,10‑四乙酸(DOTA)式(II)的制备方法。本发明的制备方法包括以下步骤：在水中，在缚酸剂的作用下，将(cyclen)式(I)与XCH2COOR进行垸基化反应；调节pH值以析出DOTA粗品；重结晶。本发明的制备方法适合于大规模工业化生产DOTA,整个过程无需采用离子交换树脂或低温冷冻方式进行纯化，产品的纯度和收率均较高。

Description

PCT国内申请，说明书已公开。

Claims (19)

  1. PCT国内申请，权利要求书已公开。
CN201780080570.8A 2016-12-30 2017-09-18 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的制备方法 Active CN110198931B (zh)

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CN2016112623356 2016-12-30
CN201611262335.6A CN108264491B (zh) 2016-12-30 2016-12-30 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的制备方法
PCT/CN2017/102056 WO2018120923A1 (zh) 2016-12-30 2017-09-18 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的制备方法

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CN110198931A true CN110198931A (zh) 2019-09-03
CN110198931B CN110198931B (zh) 2022-08-02

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CN201780080570.8A Active CN110198931B (zh) 2016-12-30 2017-09-18 1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的制备方法

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US (1) US11214553B2 (zh)
EP (1) EP3564218B1 (zh)
JP (1) JP2020504175A (zh)
KR (1) KR102265637B1 (zh)
CN (2) CN108264491B (zh)
CA (1) CA3048549C (zh)
ES (1) ES2865297T3 (zh)
MX (1) MX2019007798A (zh)
WO (1) WO2018120923A1 (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
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CN113087680A (zh) * 2020-01-08 2021-07-09 威智医药有限公司 Dota晶型及其制备方法

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CN108658882A (zh) * 2017-03-28 2018-10-16 江苏恒瑞医药股份有限公司 一种1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的制备方法
WO2021250163A1 (en) * 2020-06-10 2021-12-16 Justesa Imagen S.A.U. Procedure for obtaining gadoterate meglumine from high-purity tetraxetan (dota) and its use in the preparation of injectable galenical formulations
CN113429362A (zh) * 2021-06-01 2021-09-24 南昌大学 环胺高氯酸可逆相变材料及其制备方法
CN113956262B (zh) * 2021-10-18 2023-03-07 苏州百灵威超精细材料有限公司 一种四氮杂环烷类化合物及其中间体的合成方法

Citations (2)

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CN105939994A (zh) * 2014-02-06 2016-09-14 爱克发医疗保健公司 纯化1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸的方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113087680A (zh) * 2020-01-08 2021-07-09 威智医药有限公司 Dota晶型及其制备方法

Also Published As

Publication number Publication date
EP3564218B1 (en) 2021-02-24
ES2865297T3 (es) 2021-10-15
MX2019007798A (es) 2019-08-29
CN108264491B (zh) 2022-09-16
KR20190098236A (ko) 2019-08-21
CN110198931B (zh) 2022-08-02
US20200347023A1 (en) 2020-11-05
WO2018120923A1 (zh) 2018-07-05
KR102265637B1 (ko) 2021-06-15
US11214553B2 (en) 2022-01-04
CN108264491A (zh) 2018-07-10
CA3048549C (en) 2023-11-21
EP3564218A1 (en) 2019-11-06
EP3564218A4 (en) 2019-12-18
CA3048549A1 (en) 2018-07-05
JP2020504175A (ja) 2020-02-06

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