KR970707073A - (S)-N,N'-비스[2-히드록시-1-(히드록시메틸)에틸]-5-[(2-히드록시-1-옥소프로필)아미노]-2,4,6-트리요오도-1,3-벤젠디카복사미드의 물로부터의 결정화 방법(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) - Google Patents
(S)-N,N'-비스[2-히드록시-1-(히드록시메틸)에틸]-5-[(2-히드록시-1-옥소프로필)아미노]-2,4,6-트리요오도-1,3-벤젠디카복사미드의 물로부터의 결정화 방법(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)Info
- Publication number
- KR970707073A KR970707073A KR1019970702994A KR19970702994A KR970707073A KR 970707073 A KR970707073 A KR 970707073A KR 1019970702994 A KR1019970702994 A KR 1019970702994A KR 19970702994 A KR19970702994 A KR 19970702994A KR 970707073 A KR970707073 A KR 970707073A
- Authority
- KR
- South Korea
- Prior art keywords
- hydroxy
- ethyl
- hydroxymethyl
- alcohol
- amount
- Prior art date
Links
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 title abstract 3
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 title abstract 3
- -1 2-hydroxy-1- [(2-Hydroxy-1-Oxopropyl) Amino] -2,4,6-Triiodo-1,3-Benzenedicarboxamide Chemical compound 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 7
- 235000019441 ethanol Nutrition 0.000 claims 6
- XQZXYNRDCRIARQ-LURJTMIESA-N iopamidol Chemical compound C[C@H](O)C(=O)NC1=C(I)C(C(=O)NC(CO)CO)=C(I)C(C(=O)NC(CO)CO)=C1I XQZXYNRDCRIARQ-LURJTMIESA-N 0.000 claims 3
- 229960004647 iopamidol Drugs 0.000 claims 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims 2
- 239000007864 aqueous solution Substances 0.000 claims 2
- 230000015572 biosynthetic process Effects 0.000 claims 2
- 239000000243 solution Substances 0.000 claims 2
- 238000003786 synthesis reaction Methods 0.000 claims 2
- 150000001298 alcohols Chemical class 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000013078 crystal Substances 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract 1
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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/04—X-ray contrast preparations
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
Abstract
본 발명은 이오파미돌로 알려진 (S)-N, N'-비스〔2-히드록시-1-(히드록시메틸)에틸〕-5-〔(2-히드록시-1-옥소프로필)아미노〕-2, 4, 6-트리요오드-1, 3-벤젠디카복사미드를 물로부터 결정화하기 위한 방법에 관한 것이다. 본 발명의 방법에 따라, 약전 표준에 부합하는 결정성 무수 이오파미돌이 얻어질 수 있다.
Description
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
Claims (8)
- - 가열에 의해 탈이온수에 이오파미돌을 용해시키는 단계; - 활성탄으로 용액을 탈색시키는 단계; - 60℃에서 수용액을 진공 농축시키는 단계; - 결정화를 일으키기 위한 무수 이오파미돌의 결정체 원(germ)을 첨가하는 단계; - 60℃에서 결정화시키는 단계; - 생성된 침전물을 여과하는 단계; - 습윤 생성물을 진공 건조시키는 단계를 포함하는, 결정성 무수 형태로 이오파미돌 화합물을 제공하고 약전 표준에 부합하는 이오파미돌의 물로부터의 결정화 방법.
- 제1항에 있어서, 수용액 내의 이오파미돌의 농도가 78.6(g/mL 용액)이상인 방법.
- 제1항에 있어서, 무수 형태 이오파미돌의 결정체 원(germ)을 출발 이오파미돌 양의 1 내지 10%로 첨가하는 방법.
- 제1항에 있어서, 여과된 결정체를 선형 또는 분지(C1-C4)알콜로 더 세척하는 방법.
- 제4항에 있어서, 상기 알콜이 에틸 알콜인 방법.
- 제1항 내지 3항 중 어느 한 항의 방법에 따라 얻을 수 있는 결정체 이오파미돌에서 이전의 합성 단계로부터 유도되는 용매의 잔류량을 감소시키기 위한, 선형 또는 분지(C1-C4)알콜의 용도.
- 제1항 내지 3항 중 어느 한 항의 방법에 따라 얻을 수 있는 결정체 이오파미돌에서 이전의 합성 단계로부터 유도되는 디메틸아세타미드의 잔류량을 감소시키기 위한, 선형 또는 분지(C1-C4)알콜의 용도.
- 제7항에 있어서, 디메틸아세타미드의 양을 감소시키기 위한 에틸 알콜의 용도.※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ITRM95A000599 | 1995-09-08 | ||
| IT95RM000599 IT1277934B1 (it) | 1995-09-08 | 1995-09-08 | Processo per la cristallizzazione da acqua della s-n,n' -bis- ( 2-idrossi -1 -(idrossimetil) etil) -5- ((2 -idrossi -1- ossopropil) |
| IT95RM000831 IT1277950B1 (it) | 1995-12-19 | 1995-12-19 | Processo per la cristallizzazione da acqua della s-n,n'-bis (2-idrossi -1-(idrossimetil)etil)-5-((2-idrossi-1-ossopropil)ammino).2,4,6- |
| ITRM95A000831 | 1995-12-19 | ||
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR970707073A true KR970707073A (ko) | 1997-12-01 |
| KR100270411B1 KR100270411B1 (ko) | 2000-11-01 |
Family
ID=26332086
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1019970702994A KR100270411B1 (ko) | 1995-09-08 | 1996-08-02 | (s)-n,n'-비스[2-히드록시-1-(히드록시메틸)에틸-5-[(2-히드록시-1-옥소프로필)아미노]-2,4,6-트리요오도-1,3-벤젠디카복사미드의물로부터의결정화방법 |
Country Status (17)
| Country | Link |
|---|---|
| US (1) | US5689002A (ko) |
| EP (1) | EP0790979B1 (ko) |
| JP (1) | JP4070235B2 (ko) |
| KR (1) | KR100270411B1 (ko) |
| CN (1) | CN1070843C (ko) |
| AT (1) | ATE187437T1 (ko) |
| AU (1) | AU708195B2 (ko) |
| BR (1) | BR9606624A (ko) |
| CA (1) | CA2204734C (ko) |
| CZ (1) | CZ288645B6 (ko) |
| DE (1) | DE69605528T2 (ko) |
| ES (1) | ES2140887T3 (ko) |
| HK (1) | HK1001861A1 (ko) |
| HU (1) | HU220965B1 (ko) |
| NO (1) | NO308841B1 (ko) |
| PL (1) | PL184937B1 (ko) |
| WO (1) | WO1997009300A1 (ko) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PT101720A (pt) * | 1995-06-08 | 1997-01-31 | Hovione Sociedade Quimica S A | Processo para a purificacao e cristalizacao de iopamidol |
| KR20000031642A (ko) * | 1998-11-09 | 2000-06-05 | 강재헌 | 이오파미돌의 결정화 방법 |
| KR20050044506A (ko) * | 2001-11-16 | 2005-05-12 | 랜박시 래보러터리스 리미티드 | 결정질 이미페넴의 제조 방법 |
| CN100418945C (zh) * | 2006-01-13 | 2008-09-17 | 江苏省原子医学研究所 | 一种碘昔兰的纯化方法 |
| US20110021834A1 (en) * | 2009-07-21 | 2011-01-27 | Ge Healthcare As | Continuous process of preparing intermediate for non-ionic x-ray contrast agents |
| WO2012136813A2 (en) | 2011-04-07 | 2012-10-11 | Universitetet I Oslo | Agents for medical radar diagnosis |
| EP3548461B1 (en) | 2016-12-05 | 2021-02-03 | Bracco Imaging SpA | Mechanochemical synthesis of radiographic agents intermediates |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH608189A5 (ko) * | 1974-12-13 | 1978-12-29 | Savac Ag | |
| IL110391A (en) * | 1993-07-30 | 1998-12-06 | Zambon Spa | Process for the formation of infamidol |
-
1996
- 1996-08-02 WO PCT/EP1996/003399 patent/WO1997009300A1/en active IP Right Grant
- 1996-08-02 DE DE69605528T patent/DE69605528T2/de not_active Expired - Lifetime
- 1996-08-02 KR KR1019970702994A patent/KR100270411B1/ko not_active IP Right Cessation
- 1996-08-02 EP EP96928403A patent/EP0790979B1/en not_active Expired - Lifetime
- 1996-08-02 CN CN96191028A patent/CN1070843C/zh not_active Expired - Lifetime
- 1996-08-02 BR BR9606624A patent/BR9606624A/pt not_active Application Discontinuation
- 1996-08-02 ES ES96928403T patent/ES2140887T3/es not_active Expired - Lifetime
- 1996-08-02 HU HU9801837A patent/HU220965B1/hu unknown
- 1996-08-02 JP JP50604597A patent/JP4070235B2/ja not_active Expired - Lifetime
- 1996-08-02 AU AU67888/96A patent/AU708195B2/en not_active Expired
- 1996-08-02 CZ CZ19971385A patent/CZ288645B6/cs not_active IP Right Cessation
- 1996-08-02 PL PL96320027A patent/PL184937B1/pl unknown
- 1996-08-02 AT AT96928403T patent/ATE187437T1/de not_active IP Right Cessation
- 1996-08-02 CA CA002204734A patent/CA2204734C/en not_active Expired - Lifetime
- 1996-09-05 US US08/708,668 patent/US5689002A/en not_active Expired - Lifetime
-
1997
- 1997-04-23 NO NO971863A patent/NO308841B1/no not_active IP Right Cessation
-
1998
- 1998-02-10 HK HK98100990A patent/HK1001861A1/xx not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| MX9703341A (es) | 1997-07-31 |
| EP0790979B1 (en) | 1999-12-08 |
| HUP9801837A3 (en) | 2001-06-28 |
| CN1070843C (zh) | 2001-09-12 |
| PL320027A1 (en) | 1997-09-01 |
| DE69605528T2 (de) | 2000-05-04 |
| NO971863D0 (no) | 1997-04-23 |
| DE69605528D1 (de) | 2000-01-13 |
| EP0790979A1 (en) | 1997-08-27 |
| HK1001861A1 (en) | 1998-07-17 |
| WO1997009300A1 (en) | 1997-03-13 |
| US5689002A (en) | 1997-11-18 |
| ES2140887T3 (es) | 2000-03-01 |
| BR9606624A (pt) | 1997-11-11 |
| NO308841B1 (no) | 2000-11-06 |
| AU708195B2 (en) | 1999-07-29 |
| CA2204734C (en) | 2009-12-29 |
| PL184937B1 (pl) | 2003-01-31 |
| NO971863L (no) | 1997-04-23 |
| CZ288645B6 (cs) | 2001-08-15 |
| JPH10508878A (ja) | 1998-09-02 |
| AU6788896A (en) | 1997-03-27 |
| ATE187437T1 (de) | 1999-12-15 |
| CA2204734A1 (en) | 1997-03-13 |
| CN1164853A (zh) | 1997-11-12 |
| JP4070235B2 (ja) | 2008-04-02 |
| HUP9801837A2 (hu) | 1998-12-28 |
| KR100270411B1 (ko) | 2000-11-01 |
| HU220965B1 (hu) | 2002-07-29 |
| CZ138597A3 (cs) | 1998-02-18 |
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