SI9420046B - Postopek za kristalizacijo Iopamidola - Google Patents
Postopek za kristalizacijo Iopamidola Download PDFInfo
- Publication number
- SI9420046B SI9420046B SI9420046A SI9420046A SI9420046B SI 9420046 B SI9420046 B SI 9420046B SI 9420046 A SI9420046 A SI 9420046A SI 9420046 A SI9420046 A SI 9420046A SI 9420046 B SI9420046 B SI 9420046B
- Authority
- SI
- Slovenia
- Prior art keywords
- lopamidol
- solvent
- butanol
- sec
- purified
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C237/00—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups
- C07C237/28—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups having the carbon atom of at least one of the carboxamide groups bound to a carbon atom of a non-condensed six-membered aromatic ring of the carbon skeleton
- C07C237/46—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups having the carbon atom of at least one of the carboxamide groups bound to a carbon atom of a non-condensed six-membered aromatic ring of the carbon skeleton having carbon atoms of carboxamide groups, amino groups and at least three atoms of bromine or iodine, bound to carbon atoms of the same non-condensed six-membered aromatic ring
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Claims (33)
1 PATENTNI ZAHTEVKI 1. Postopek za čiščenje L-5-a-hidroksipropionilamino-2,4,6-triiodo-isoftalne kisline bis-(1,3-dihidroksiizopropilamida) (lopamidol), ki vsebuje naslednja koraka: topljenje surove trdne oblike lopamidola v topilu, izbranem iz skupine sestavljene iz n-butanola, sec-butanola, izobutanola, t-butanola in njihovih mešanic; in kristalizacijo čistega lopamidola iz tega, kjer ima omenjeni čisti lopamidol manjši ostanek topila kot ta surov lopamidol.
2. Postopek po zahtevku 1, kjer je teža lopamidola proti volumnu topila 3 proti 20.
3. Postopek po zahtevku 1, pri katerem je to topilo n-butanol.
4. Postopek po zahtevku 1, pri katerem je to topilo sec-butanol.
5. Postopek po zahtevku 1, pri katerem je to topilo izobutanol.
6. Postopek po zahtevku 1, pri katerem je to topilo t-butanol.
7. Postopek za čiščenje L-5-a-hidroksipropionilamino-2,4,6-triiodo-isoftalne kisline bis-(1,3-dihidroksiizopropilamida) (lopamidol), ki vsebuje naslednje korake: 2 obdelava vodne raztopine lopamidola s topilom, izbranim iz skupine, sestavljene iz n-butanola, sec-butanola, izobutanola, t-butanola in mešanic le-teh za pridobitev mešanice vsebujoče lopamidol; in kristalizacijo čistega lopamidola od tam, s topljenjem čistega trdnega lopamidola v topilu, vsebujoč n-butanol, sec-butanol, izobutanol, t-butanol in mešanice le-teh; in kristalizacijo čistega lopamidola iz tega, kjer ima omenjeni čisti lopamidol manjši ostanek topila kot ta surov lopamidol.
8. Postopek po zahtevku 7, pri katerem je to topilo n-butanol.
9. Postopek po zahtevku 7, pri katerem je to topilo sec-butanol.
10. Postopek po zahtevku 7, pri katerem je to topilo izobutanol.
11. Postopek po zahtevku 7, pri katerem je to topilo t-butanol.
12. Postopek po zahtevku 7, pri katerem omenjena vodna raztopina lopamidola izhaja iz predhodnih stopenj sinteze ali čiščenja produkta.
13. Postopek po zahtevku 7, kjer omenjen korak postopka vsebuje dodajanje tega topila k omenjeni vodni raztopini vsebujoči lopamidol za formiranje omenjene mešanice vsebujoče lopamidol in destiliranje te mešanice za delno ali popolno odstranitev prisotne vode. 3
14. Postopek po zahtevku 7, ki nadalje vsebuje korak za obdelavo omenjene mešanice vsebujoče lopamidol s tretjim topilom za pridobitev trojnih azeotropov.
15. Postopek po zahtevku 14, pri katerem je to tretje topilo toluen.
16. Očiščen L-5-a-hidroksipropionilamino-2,4,6-triiodo-isoftalne kisline bis-(1,3-dihidroksiizopropilamida) (lopamidol), pripravljen s pomočjo postopka, ki vsebuje topljenje surove trdne oblike lopamidola v topilu, izbranem iz skupine sestavljene iz n-butanola, sec-butanola, izobutanola, t-butanola in njihovih mešanic; in kristalizacijo čistega lopamidola iz tega, kjer ima omenjeni čisti lopamidol manjši ostanek topila kot ta surov lopamidol.
17. Ne-ionski kontrastni medij vsebujoč L-5-a-hidroksipropionilamino-2,4,6-triiodo-isofitalne kisline bis-(1,3-dihidiOksiizopropilamida) (lopamidol), očiščen s: topljenjem surovega trdnega lopamidola v topilu, izbranem iz skupine, sestavljene iz n-butanola, sec-butanola, izobutanola, t-butanola in mešanic le-teh; in 4 kristalizacijo čistega lopamidola iz tega, kjer ima omenjeni čisti lopamidol manjši ostanek topila kot ta surov lopamidol.
18. Ne-ionski kontrastni medij vsebujoč L-5-a-hidroksipropionilamino-2,4,6-triiodo-isoftalne kisline bis-(1,3-dihidroksiizopropilamida) (lopamidol), očiščen s: obdelavo vodne raztopine lopamidola s topilom, izbranim iz skupine, sestavljene iz n-butanola, sec-butanola, izobutanola, t-butanola in mešanic le-teh za pridobitev mešanice vsebujoče lopamidol; in kristalizacijo čistega lopamidola iz tega, kjer ima omenjeni čisti lopamidol manjši ostanek topila kot ta surov lopamidol.
19. Očiščen lopamidol po zahtevku 16, ki vsebuje manj ali enako 2000 ppm ostanka topila.
20. Očiščen lopamidol po zahtevku 16, ki vsebuje manj ali enako 1300 ppm ostanka topila.
21. Ne-ionski kontrastni medij po zahtevku 17, kjer očiščen lopamidol vsebuje manj ali enako 2000 ppm ostanka topila. 5
22. Ne-ionski kontrastni medij po zahtevku 17, kjer očiščen lopamidol vsebuje manj ali enako 1300 ppm ostanka topila.
23. Ne-ionski kontrastni medij po zahtevku 18, kjer očiščen lopamidol vsebuje manj ali enako 2000 ppm ostanka topila.
24. Ne-ionski kontrastni medij po zahtevku 18, kjer očiščen lopamidol vsebuje manj ali enako 1300 ppm ostanka topila.
25. Očiščen lopamidol po zahtevku 16, kjer je topilo sec-butanol.
26. Ne-ionski kontrastni medij po zahtevku 17, kjer je topilo sec-butanol.
27. Ne-ionski kontrastni medij po zahtevku 18, kjer je topilo sec-butanol.
28. Očiščen lopamidol po zahtevku 19, kjer je topilo sec-butanol.
29. Očiščen lopamidol po zahtevku 20, kjer je topilo sec-butanol.
30. Ne-ionski kontrastni medij po zahtevku 21, kjer je topilo sec-butanol.
31. Ne-ionski kontrastni medij po zahtevku 22, kjer je topilo sec-butanol.
32. Ne-ionski kontrastni medij po zahtevku 23, kjer je topilo sec-butanol.
33. Ne-ionski kontrastni medij po zahtevku 24, kjer je topilo sec-butanol. Za: BRACCO INTERNATIONAL B.V.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ITMI931720A IT1257001B (it) | 1993-07-30 | 1993-07-30 | Processo per la cristalizzazione dello iopamidolo |
| IT000760 IT1269339B (it) | 1994-04-20 | 1994-04-20 | Processo per la cristallizzazione dello iopamidolo |
| PCT/EP1994/002415 WO1995004031A1 (en) | 1993-07-30 | 1994-07-22 | Process for the crystallization of iopamidol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| SI9420046A SI9420046A (en) | 1996-10-31 |
| SI9420046B true SI9420046B (sl) | 2003-10-31 |
Family
ID=26331032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SI9420046A SI9420046B (sl) | 1993-07-30 | 1994-07-22 | Postopek za kristalizacijo Iopamidola |
Country Status (29)
| Country | Link |
|---|---|
| US (3) | US5571941A (sl) |
| JP (1) | JP3299045B2 (sl) |
| KR (1) | KR100355211B1 (sl) |
| CN (1) | CN1035940C (sl) |
| AT (1) | AT404832B (sl) |
| AU (1) | AU690138B2 (sl) |
| BE (1) | BE1008403A4 (sl) |
| CA (1) | CA2128942C (sl) |
| CH (1) | CH686783A5 (sl) |
| CZ (1) | CZ289300B6 (sl) |
| DE (1) | DE4426818A1 (sl) |
| DK (1) | DK172074B1 (sl) |
| ES (1) | ES2102312B1 (sl) |
| FI (1) | FI960400A (sl) |
| FR (1) | FR2708601B1 (sl) |
| GB (1) | GB2280436B (sl) |
| GR (1) | GR940100366A (sl) |
| HU (1) | HU217023B (sl) |
| IE (1) | IE80675B1 (sl) |
| IL (1) | IL110391A (sl) |
| NL (1) | NL194272C (sl) |
| NO (1) | NO304226B1 (sl) |
| NZ (1) | NZ271632A (sl) |
| PT (1) | PT101554B (sl) |
| RU (1) | RU2135462C1 (sl) |
| SE (1) | SE9402595L (sl) |
| SI (1) | SI9420046B (sl) |
| WO (1) | WO1995004031A1 (sl) |
| ZA (1) | ZA945472B (sl) |
Families Citing this family (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IL110391A (en) | 1993-07-30 | 1998-12-06 | Zambon Spa | Process for the formation of infamidol |
| US6310243B1 (en) * | 1994-09-23 | 2001-10-30 | Nycomed Imaging As | Iodinated x-ray contrast media |
| PT101720A (pt) * | 1995-06-08 | 1997-01-31 | Hovione Sociedade Quimica S A | Processo para a purificacao e cristalizacao de iopamidol |
| AU6516196A (en) * | 1995-07-04 | 1997-02-05 | Recordati S.A. | A process for preparing iopamidol by using a c1-c5 monoalkylether of a c2-c10 alkylene-glycol |
| AU708195B2 (en) * | 1995-09-08 | 1999-07-29 | Bracco International B.V. | 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 |
| PT101919B (pt) * | 1996-09-30 | 2000-01-31 | Hovione Sociedade Quimica Sa | Um processo para a purificacao de tohexol |
| KR100758741B1 (ko) * | 1997-02-11 | 2007-09-14 | 브라코 인터내셔날 비이.브이. | 선형 또는 분지형 (ｃ5-ｃ6) 알콜 또는 그의 혼합물로부터 (ｓ)-ｎ,ｎ'-비스[2-히드록시-1-(히드록시메틸)에틸]-5-[(2-히드록시-1-옥소프로필)아미노]-2,4,6-트리요오도-1,3-벤젠디카르복스아미드의 결정화 방법 |
| GB9720969D0 (en) * | 1997-10-02 | 1997-12-03 | Nycomed Imaging As | Process |
| KR20000031642A (ko) * | 1998-11-09 | 2000-06-05 | 강재헌 | 이오파미돌의 결정화 방법 |
| US6265610B1 (en) | 1999-01-12 | 2001-07-24 | The University Of North Carolina At Chapel Hill | Contrast media for angiography |
| US6803485B2 (en) | 1999-02-26 | 2004-10-12 | Bracco Imaging S.P.A. | Process for the preparation of iopamidol |
| IT1319671B1 (it) | 2000-12-01 | 2003-10-23 | Bracco Spa | Processo per la preparazione di (s)-n,n'-bis(2-idrossi-1-(idrossimetil)etil)-5-((2-idrossi-1-ossopropil)ammino) |
| DE102005059191B4 (de) * | 2005-12-05 | 2008-02-07 | Bayer Schering Pharma Ag | Verfahren zur Rückgewinnung von für pharmazeutische Zwecke geeignetem Iopromid aus Mutterlaugen |
| KR100976097B1 (ko) | 2008-12-05 | 2010-08-16 | 주식회사 대웅제약 | 이오프로마이드의 ｚ 이성체를 선택적으로 결정화하는 방법 |
| CA2757480A1 (en) * | 2009-04-02 | 2010-10-07 | Allergan, Inc. | Prostaglandin e receptor antagonists |
| WO2012136813A2 (en) | 2011-04-07 | 2012-10-11 | Universitetet I Oslo | Agents for medical radar diagnosis |
| DE102012104679A1 (de) | 2011-05-30 | 2012-12-06 | Westfälische Wilhelms-Universität Münster | Biotechnologische konversion von glycerin zu 2-amino-1,3-propandiol (serinol) in rekombinanten escherichia coli |
| CA2890449C (en) | 2012-12-19 | 2020-12-29 | Ge Healthcare As | Purification of x-ray contrast agents |
| KR102128423B1 (ko) * | 2018-09-17 | 2020-07-01 | (주)유케이케미팜 | 조영제 이오메프롤의 제조방법 |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH608189A5 (sl) * | 1974-12-13 | 1978-12-29 | Savac Ag | |
| GB1548594A (en) * | 1976-06-11 | 1979-07-18 | Nyegaard & Co As | Triiodoisophthalic acid amides |
| IT1193211B (it) * | 1979-08-09 | 1988-06-15 | Bracco Ind Chimica Spa | Derivati dell'acido 2,4,6-triiodo-isoftalico,metodo per la loro preparazione e mezzi di contrasto che li contengono |
| DE3150916A1 (de) * | 1981-12-18 | 1983-06-30 | Schering Ag, 1000 Berlin Und 4619 Bergkamen | N-hydroxyaethylierte 2,4,6-trijodaminoisiophthalsaeure-bis- trihydroxybutylamide, deren herstellung und diese enthaltende roentgenkontrastmittel" |
| US5204086A (en) * | 1982-10-01 | 1993-04-20 | Nycomed Imaging As | X-ray contrast agent |
| ATE79368T1 (de) * | 1987-05-22 | 1992-08-15 | Bracco Spa | Herstellung von 5-acylamino-2,4,6-trijodo- oder tribromo-benzoesaeure-derivate. |
| IT1248741B (it) * | 1991-02-26 | 1995-01-26 | Bracco Spa | Processo di concentrazione e di purificazione di composti organici |
| IL110391A (en) | 1993-07-30 | 1998-12-06 | Zambon Spa | Process for the formation of infamidol |
-
1994
- 1994-07-20 IL IL11039194A patent/IL110391A/en not_active IP Right Cessation
- 1994-07-22 SI SI9420046A patent/SI9420046B/sl unknown
- 1994-07-22 CN CN94192930A patent/CN1035940C/zh not_active Expired - Lifetime
- 1994-07-22 GR GR940100366A patent/GR940100366A/el unknown
- 1994-07-22 NZ NZ271632A patent/NZ271632A/en not_active IP Right Cessation
- 1994-07-22 HU HU9600191A patent/HU217023B/hu unknown
- 1994-07-22 WO PCT/EP1994/002415 patent/WO1995004031A1/en active Application Filing
- 1994-07-22 RU RU96105070A patent/RU2135462C1/ru active
- 1994-07-22 KR KR1019960700580A patent/KR100355211B1/ko not_active IP Right Cessation
- 1994-07-22 AU AU75321/94A patent/AU690138B2/en not_active Expired
- 1994-07-25 ZA ZA945472A patent/ZA945472B/xx unknown
- 1994-07-25 GB GB9414912A patent/GB2280436B/en not_active Expired - Lifetime
- 1994-07-26 FR FR9409238A patent/FR2708601B1/fr not_active Expired - Lifetime
- 1994-07-26 CH CH02354/94A patent/CH686783A5/it not_active IP Right Cessation
- 1994-07-26 PT PT101554A patent/PT101554B/pt not_active IP Right Cessation
- 1994-07-26 NL NL9401229A patent/NL194272C/nl not_active IP Right Cessation
- 1994-07-27 CA CA002128942A patent/CA2128942C/en not_active Expired - Lifetime
- 1994-07-28 DE DE4426818A patent/DE4426818A1/de not_active Ceased
- 1994-07-29 AT AT0150594A patent/AT404832B/de not_active IP Right Cessation
- 1994-07-29 IE IE940609A patent/IE80675B1/en not_active IP Right Cessation
- 1994-07-29 JP JP17811594A patent/JP3299045B2/ja not_active Expired - Lifetime
- 1994-07-29 DK DK089294A patent/DK172074B1/da not_active IP Right Cessation
- 1994-07-29 US US08/281,985 patent/US5571941A/en not_active Ceased
- 1994-07-29 ES ES09401679A patent/ES2102312B1/es not_active Expired - Fee Related
- 1994-07-29 BE BE9400717A patent/BE1008403A4/fr not_active IP Right Cessation
- 1994-07-29 SE SE9402595A patent/SE9402595L/xx not_active Application Discontinuation
- 1994-07-29 CZ CZ19941831A patent/CZ289300B6/cs not_active IP Right Cessation
-
1996
- 1996-01-29 NO NO960376A patent/NO304226B1/no not_active IP Right Cessation
- 1996-01-29 FI FI960400A patent/FI960400A/fi not_active Application Discontinuation
-
1997
- 1997-02-07 US US08/797,610 patent/USRE36433E/en not_active Expired - Lifetime
-
1998
- 1998-08-25 US US09/139,894 patent/US6506938B1/en not_active Expired - Lifetime
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