AR081271A1 - PREPARATION OF GADOBUTROL THROUGH CERAMIC MEMBRANE - Google Patents

PREPARATION OF GADOBUTROL THROUGH CERAMIC MEMBRANE

Info

Publication number
AR081271A1
AR081271A1 ARP100104103A AR081271A1 AR 081271 A1 AR081271 A1 AR 081271A1 AR P100104103 A ARP100104103 A AR P100104103A AR 081271 A1 AR081271 A1 AR 081271A1
Authority
AR
Argentina
Prior art keywords
lithium
preparation
complex
dioxepan
dialysis
Prior art date
Application number
Other languages
Spanish (es)
Inventor
Johannes Platzek
Original Assignee
Bayer Schering Pharma Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE200910053252 external-priority patent/DE102009053252B3/en
Priority claimed from DE200910057274 external-priority patent/DE102009057274B4/en
Application filed by Bayer Schering Pharma Ag filed Critical Bayer Schering Pharma Ag
Publication of AR081271A1 publication Critical patent/AR081271A1/en

Links

Classifications

    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

Se describe un procedimiento para la preparacion de gadobutrol que proporciona el compuesto meta a partir de complejo de N-(6-hidroxi-2, 2-dimetil-1,3-dioxepan-5-il)-1,4,7,10-tetraaza-ciclododecan-litio en un proceso en un recipiente, sin aislamiento intermedio y purificacion intermedia de productos intermediarios, por medio de diálisis a través de membranas cerámicas con gran rendimiento y pureza. Reivindicacion 1: Procedimiento para la preparacion del complejo de gadolinio del N-(1- hidroximetil-2,3-dihidroxipropil)-1,4,7-triscarboximetil-1,4,7,10-tetra-azaciclododecano ôgadobutrolö, en el que se hace reaccionar complejo de cloruro de litio o bromuro de Iitio-N-(6-hidroxi-2,2-dimetil-1,3-dioxepan-5-il)-1,4 7,10-tetraaza-ciclododecano en solventes polares con ácido haloacético e hidroxido de litio o N-metil-imidazol, luego se acidifica, se lleva a cabo una determinacion del contenido en ligando de butrol y se anade la cantidad estequiométrica de una sal de gadolinio, se agita y por posterior adicion de hidroxido de litio o N-metil-imidazol se regula a un rango pH de 4-8, luego se dializa en una instalacion de ultrafiltracion a través de una membrana cerámica con un corte de M = 100-400, se enjuaga con agua pura, una vez alcanzado un determinado valor de conductividad por medio de diálisis se concentra y se recristaliza.A process for the preparation of gadobutrol which provides the target compound from N- (6-hydroxy-2,2-dimethyl-1,3-dioxepan-5-yl) -1,4,7,10 complex is described. -tratraza-cyclododecan-lithium in a process in a container, without intermediate isolation and intermediate purification of intermediate products, by means of dialysis through ceramic membranes with great performance and purity. Claim 1: Process for the preparation of the gadolinium complex of N- (1- hydroxymethyl-2,3-dihydroxypropyl) -1,4,7-triscarboxymethyl-1,4,7,10-tetra-azacyclododecane ôgadobutrolö, wherein Lithium chloride complex or Iitio-N- (6-hydroxy-2,2-dimethyl-1,3-dioxepan-5-yl) -1,4 7,10-tetraaza-cyclododecane bromide is reacted in polar solvents with haloacetic acid and lithium hydroxide or N-methyl-imidazole, then acidified, a determination of the butrol ligand content is carried out and the stoichiometric amount of a gadolinium salt is added, stirred and subsequently added by hydroxide of lithium or N-methyl-imidazole is regulated to a pH range of 4-8, then dialyzed in an ultrafiltration facility through a ceramic membrane with a cut of M = 100-400, rinsed with pure water, a Once a certain conductivity value has been reached through dialysis, it is concentrated and recrystallized.

ARP100104103 2009-11-09 2010-11-05 PREPARATION OF GADOBUTROL THROUGH CERAMIC MEMBRANE AR081271A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200910053252 DE102009053252B3 (en) 2009-11-09 2009-11-09 Making gadobutrol, to diagnose stroke, comprises e.g. reacting N-(6-hydroxy-2,2-dimethyl-1,3-dioxepan-5-yl)-tetraaza-cyclododecane lithium chloride or bromide complex with haloacetic acid and lithium hydroxide or N-methyl imidazole
DE200910057274 DE102009057274B4 (en) 2009-12-02 2009-12-02 Gadobutrol preparation using trioxobicyclo-octane

Publications (1)

Publication Number Publication Date
AR081271A1 true AR081271A1 (en) 2012-08-01

Family

ID=43708819

Family Applications (1)

Application Number Title Priority Date Filing Date
ARP100104103 AR081271A1 (en) 2009-11-09 2010-11-05 PREPARATION OF GADOBUTROL THROUGH CERAMIC MEMBRANE

Country Status (4)

Country Link
AR (1) AR081271A1 (en)
TW (1) TW201139388A (en)
UY (1) UY33015A (en)
WO (1) WO2011054480A1 (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009053171B4 (en) * 2009-11-04 2011-07-21 Bayer Schering Pharma Aktiengesellschaft, 13353 Process for the preparation of the calcium complex of dihydroxy-hydroxy-methylpropyl-tetraazacyclododecane-triacetic acid (Calcobutrol)
PE20141325A1 (en) 2011-04-21 2014-10-08 Bayer Ip Gmbh HIGH PURITY GADOBUTROL PREPARATION
WO2015117911A1 (en) 2014-02-06 2015-08-13 Agfa Healthcare Process for purifying 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid
CN106187930B (en) * 2016-07-12 2018-10-19 嘉实（湖南）医药科技有限公司 The preparation method of high-purity calcobutrol
CN106543094A (en) * 2016-11-04 2017-03-29 嘉实（湖南）医药科技有限公司 The preparation method of high-purity gadobutrol
CN109293592A (en) * 2017-07-24 2019-02-01 天津科伦药物研究有限公司 A method of preparing Gadobutrol
CN113527223B (en) * 2021-06-22 2023-05-09 安徽普利药业有限公司 Refining method of gadobutrol

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3625417C2 (en) 1986-07-28 1998-10-08 Schering Ag Tetraazacyclododecane derivatives
DE4009119A1 (en) 1990-03-19 1991-09-26 Schering Ag 1,4,7,10-TETRAAZACYCLODODECANE-BUTYLTRIOLS, METHOD FOR THE PRODUCTION THEREOF AND PHARMACEUTICAL AGENTS CONTAINING THEM
US5447635A (en) 1991-02-26 1995-09-05 Bracco International B.V. Process of concentration and purification of organic compounds
DE19724186C2 (en) 1997-06-02 2002-07-18 Schering Ag Process for the mono- and 1,7-bis-N-ß-hydroxyalkylation of cycles and the corresponding N-ß-hydroxyalkyl-1,4,7,10-tetraazacyclododecane-Li salt complexes
IT1292128B1 (en) 1997-06-11 1999-01-25 Bracco Spa PROCESS FOR THE PREPARATION OF MACROCYCLIC CHELANTS AND THEIR CHELATES WITH PARAMAGNETIC METALLIC IONS
DE10064467C2 (en) * 2000-12-15 2002-10-31 Schering Ag Lithium complexes of N- (1-hydroxymethyl-2,3-dihydroxypropyl) -1,4,7-triscarboxymethyl-1,4,7,10-tetraazacyclododecane, their preparation and use
DE102004006048B4 (en) * 2004-02-02 2009-11-26 Axxonis Pharma Ag An intravenous injection or infusion solution containing a combination drug for use as a contrast enhancer in MR angiography

Also Published As

Publication number Publication date
UY33015A (en) 2011-06-30
TW201139388A (en) 2011-11-16
WO2011054480A1 (en) 2011-05-12

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