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IT1277950B1 - Prepn. of crystalline, anhydrous Iopamidol - by crystallisation from deionised water, useful as X=ray contrast agent - Google Patents

Prepn. of crystalline, anhydrous Iopamidol - by crystallisation from deionised water, useful as X=ray contrast agent

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Publication number
IT1277950B1
IT1277950B1 ITRM950831A IT1277950B1 IT 1277950 B1 IT1277950 B1 IT 1277950B1 IT RM950831 A ITRM950831 A IT RM950831A IT 1277950 B1 IT1277950 B1 IT 1277950B1
Authority
IT
Italy
Prior art keywords
solution
crystallisation
crystalline
deionised water
prepn
Prior art date
Application number
Other languages
Italian (it)
Inventor
Marina Mauro
Original Assignee
Fructamine Spa
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
Application filed by Fructamine Spa filed Critical Fructamine Spa
Publication of ITRM950831A0 publication Critical patent/ITRM950831A0/it
Priority to IT95RM000831 priority Critical patent/IT1277950B1/en
Priority to CN96191028A priority patent/CN1070843C/en
Priority to AU67888/96A priority patent/AU708195B2/en
Priority to CA002204734A priority patent/CA2204734C/en
Priority to HU9801837A priority patent/HU220965B1/en
Priority to DE69605528T priority patent/DE69605528T2/en
Priority to CZ19971385A priority patent/CZ288645B6/en
Priority to PL96320027A priority patent/PL184937B1/en
Priority to HK98100990.3A priority patent/HK1001861B/en
Priority to ES96928403T priority patent/ES2140887T3/en
Priority to EP96928403A priority patent/EP0790979B1/en
Priority to KR1019970702994A priority patent/KR100270411B1/en
Priority to PCT/EP1996/003399 priority patent/WO1997009300A1/en
Priority to AT96928403T priority patent/ATE187437T1/en
Priority to JP50604597A priority patent/JP4070235B2/en
Priority to BR9606624A priority patent/BR9606624A/en
Priority to US08/708,668 priority patent/US5689002A/en
Priority to NO971863A priority patent/NO308841B1/en
Priority to MXPA/A/1997/003341A priority patent/MXPA97003341A/en
Publication of ITRM950831A1 publication Critical patent/ITRM950831A1/en
Application granted granted Critical
Publication of IT1277950B1 publication Critical patent/IT1277950B1/en

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Process (I) for the crystallisation of Iopamidol ((S)-N,N'-bis(2-hydroxy-1- (hydroxymethyl)ethyl)-5- ((2-hydroxy-1-oxopropyl)amino)- 2,4,6-triiodo-1,3-benzenedicarboxamide) (II) from water to afford a crystalline anhydrous form of pharmacopoeia standard involves: (a) dissolving (II) in deionised water by heating; (b) decolourising the solution with active carbon; (c) concn. of the aq. solution in vacuo at 60[deg]C; (d) seeding the hot solution with anhydrous (II); (e) crystallising at 60[deg]C; (f) filtering the ppte; and (g) drying the wet product in vacuo. The use of a 1-4C alcohol to reduce the residual content of reaction solvents in the crystals is also claimed. The aq. solution in step (a) is pref. satd. i.e. contg. > 78.6 g (II)/ml of solution and the amt. of seed crystals added in step (d) is 1-10% of the crude (II). To reduce the content of reaction solvents esp. dimethylacetamide deriving from the previous synthetic steps, the filtered crystals are washed with pref. EtOH.
IT95RM000831 1995-09-08 1995-12-19 Prepn. of crystalline, anhydrous Iopamidol - by crystallisation from deionised water, useful as X=ray contrast agent IT1277950B1 (en)

Priority Applications (19)

Application Number Priority Date Filing Date Title
IT95RM000831 IT1277950B1 (en) 1995-12-19 1995-12-19 Prepn. of crystalline, anhydrous Iopamidol - by crystallisation from deionised water, useful as X=ray contrast agent
EP96928403A EP0790979B1 (en) 1995-09-08 1996-08-02 Process for the crystallization from water of (s)-n,n'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[(2-hydroxy-1-oxopropyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamide
PCT/EP1996/003399 WO1997009300A1 (en) 1995-09-08 1996-08-02 Process for the crystallization from water of (s)-n,n'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[(2-hydroxy-1-oxopropyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamide
CA002204734A CA2204734C (en) 1995-09-08 1996-08-02 Process for the crystallization from water of (s)-n,n'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[(2-hydroxy-1-oxopropyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamide
HU9801837A HU220965B1 (en) 1995-09-08 1996-08-02 Process for the crystallization from water of (s)-n,n'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[(2-hydroxy-1-oxopropyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamide
DE69605528T DE69605528T2 (en) 1995-09-08 1996-08-02 METHOD FOR CRYSTALLIZING FROM WATER OF (S) -N, N'-BIS [2-HYDROXY-1- (HYDROXYMETHIEL) ETHYL] -5 - [(2-HYDROXY-1-OXOPROPYL) AMINO] -2,4,6- TRIIODO-1,3-BENZOLDICARBOXAMIDE
CZ19971385A CZ288645B6 (en) 1995-09-08 1996-08-02 Crystallization process of Iopamidol
PL96320027A PL184937B1 (en) 1995-09-08 1996-08-02 Method of crystallising s)-n,n'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[2-hydroxy-1-oxypropyl)amino]2,4,6-triiodine-1,3-benzenodicarboxyamide from aquepus solution
HK98100990.3A HK1001861B (en) 1995-09-08 1996-08-02 Process for the crystallization from water of (s)-n,n'-bis[2-hydroxy-1-(hydroxymethyl)ethyl]-5-[(2-hydroxy-1-oxopropyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamide
ES96928403T ES2140887T3 (en) 1995-09-08 1996-08-02 PROCEDURE FOR CRYSTALLIZING IN WATER (S) -N-N'-BIS (2-HIDROXI-1- (HIDROXIMETIL) ETIL) -5 - ((2-HIDROXI-1-OXOPROPIL) AMINO) -2,4,6-TRIYODO -1,3-BENZENODICARBOXAMIDE.
CN96191028A CN1070843C (en) 1995-09-08 1996-08-02 Process for crystallization from water of (S)-N,N'-bis[2-hydroxy-1-(hydroxymethyl) ethyl]-5-[(2-hydroxy-1-oxopropyl)amino]-2,4,6-triiodo-1,3-benzendicarboxamide
KR1019970702994A KR100270411B1 (en) 1995-09-08 1996-08-02 Process for the Crystallization from Water of (S)-N,N'-Bis[2-Hydroxy-1-(Hydroxymethyl)Ethyl]-5-[(2-Hydroxy-1-Oxopropyl)Amino]-2,4,6-Triiodo-1,3-Benzendicarboxamide
AU67888/96A AU708195B2 (en) 1995-09-08 1996-08-02 Process for the crystallization from water of (S)-N,N'-bis{2-hydroxy-1-(hydroxymethyl)ethyl}-5-{(2-hydroxy -1-oxopropyl)amino}-2,4,6-triiodo-1,3-benzendicarboxamide
AT96928403T ATE187437T1 (en) 1995-09-08 1996-08-02 METHOD FOR CRYSTALLIZATION FROM WATER OF (S)-N,N'-BIS(2-HYDROXY-1-(HYDROXYMETHIEL)ETHYL>5-((2-HYDROXY-1-OXOPROPYL)AMINO>-2,4,6-TRIIODO - ,3- BENZOLDICARBOXAMIDE
JP50604597A JP4070235B2 (en) 1995-09-08 1996-08-02 (S) -N, N′-bis [2-hydroxy-1- (hydroxymethyl) ethyl] -5-[(2-hydroxy-1-oxopropyl) amino] -2,4,6-triiodo-1, Method for crystallizing 3-benzenedicarboxamide from water
BR9606624A BR9606624A (en) 1995-09-08 1996-08-02 Process for the crystallization of (s) -n, n'-bisÚ2-hydroxy-1- (hydroxymethyl) ethyl¾-5-Ú (2-hydroxy-1-oxopropyl) amino¾-2,4,6-triiodo-1,3 -benzonodicar-boxamide from water
US08/708,668 US5689002A (en) 1995-09-08 1996-09-05 Process for the crystallization from water of (S)-N,N'-bis 2-hydroxy-1-(hydroxymethyl)ethyl!-5- 2-hydroxy-1-oxopropyl)amino!-2,4,6-triiodo-1,3-benzendicarboxamide
NO971863A NO308841B1 (en) 1995-09-08 1997-04-23 Process for the crystallization of (S) -N, N'-bis [2-hydroxy-1- (hydroxymethyl) ethyl] -5 [(2-hydroxy-1-oxopropyl) amino] -2,4,6-triiodo-1 , 3-benzenedicarboxamide from water, and uses of (C1-C4 alcohols)
MXPA/A/1997/003341A MXPA97003341A (en) 1995-09-08 1997-05-07 Process for the crystallization of (s) -n, n'-bis [2-hydroxy-1- (hydroxymethyl) ethyl] -5 - [(2-hydroxy-1-oxopropyl) amino] -2,4,6-triyodo -1,3-bencendicarboxamide from a

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
IT95RM000831 IT1277950B1 (en) 1995-12-19 1995-12-19 Prepn. of crystalline, anhydrous Iopamidol - by crystallisation from deionised water, useful as X=ray contrast agent

Publications (3)

Publication Number Publication Date
ITRM950831A0 ITRM950831A0 (en) 1995-12-19
ITRM950831A1 ITRM950831A1 (en) 1997-06-19
IT1277950B1 true IT1277950B1 (en) 1997-11-12

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ID=11403721

Family Applications (1)

Application Number Title Priority Date Filing Date
IT95RM000831 IT1277950B1 (en) 1995-09-08 1995-12-19 Prepn. of crystalline, anhydrous Iopamidol - by crystallisation from deionised water, useful as X=ray contrast agent

Country Status (1)

Country Link
IT (1) IT1277950B1 (en)

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Publication number Publication date
ITRM950831A0 (en) 1995-12-19
ITRM950831A1 (en) 1997-06-19

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