KR101051534B1 - 실리카 겔을 이용한 n-치환 말레이미드의 정제방법 - Google Patents
실리카 겔을 이용한 n-치환 말레이미드의 정제방법 Download PDFInfo
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- KR101051534B1 KR101051534B1 KR1020070104593A KR20070104593A KR101051534B1 KR 101051534 B1 KR101051534 B1 KR 101051534B1 KR 1020070104593 A KR1020070104593 A KR 1020070104593A KR 20070104593 A KR20070104593 A KR 20070104593A KR 101051534 B1 KR101051534 B1 KR 101051534B1
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- silica gel
- substituted maleimide
- gel column
- purifying
- maleimide
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/44—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having three double bonds between ring members or between ring members and non-ring members
- C07D207/444—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having three double bonds between ring members or between ring members and non-ring members having two doubly-bound oxygen atoms directly attached in positions 2 and 5
- C07D207/448—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having three double bonds between ring members or between ring members and non-ring members having two doubly-bound oxygen atoms directly attached in positions 2 and 5 with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms, e.g. maleimide
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/40—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having five-membered rings with one nitrogen as the only ring hetero atom, e.g. sulpiride, succinimide, tolmetin, buflomedil
- A61K31/4015—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having five-membered rings with one nitrogen as the only ring hetero atom, e.g. sulpiride, succinimide, tolmetin, buflomedil having oxo groups directly attached to the heterocyclic ring, e.g. piracetam, ethosuximide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/12—Unsaturated polyimide precursors
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Epidemiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Pharmacology & Pharmacy (AREA)
- Pest Control & Pesticides (AREA)
- Animal Behavior & Ethology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Pyrrole Compounds (AREA)
Abstract
Description
Claims (12)
- 말레산 무수물과 1차 아민의 반응에 의하여 제조되는 비극성 용매 존재 하의 N-치환 말레이미드의 정제방법에 있어서,N-치환 말레이미드 용액을 실리카 겔 컬럼에 통과시키되, 상기 N-치환 말레이미드 용액의 부피가 상기 실리카 겔 부피 대비 1.5배를 넘지 않도록 하여 상기 실리카 겔 컬럼에 붉은 색의 불순물을 흡착시키는 단계, 및비극성 용매를 상기 실리카 겔 컬럼에 통과시킴으로써 상기 실리카 겔에 흡착된 N-치환 말레이미드를 용출시켜 상기 실리카 겔 컬럼으로부터 분리하는 단계,를 포함하는N-치환 말레이미드의 정제방법.
- 제 1 항에 있어서,극성 용매를 상기 실리카 겔 컬럼에 통과시킴으로써 상기 실리카 겔에 흡착된 상기 불순물을 용출시켜 상기 실리카 겔 컬럼으로부터 분리하고 상기 실리카 겔 컬럼을 재생하는 단계를 더 포함하는 것을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 2 항에 있어서,상기 극성 용매는 아세톤, 테트라하이드로퓨란, 디메틸포름아마이드 또는 이들의 혼합 용매인 것을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 2 항에 있어서,상기 극성 용매는 아세톤이고, 사용되는 상기 극성용매의 부피는 상기 실리카 겔 부피와 동일한 것임을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 1 항에 있어서,상기 비극성 용매는 톨루엔, 크실렌, 벤젠, 에틸벤젠, 쿠멘, 메시틸렌, t-브틸 벤젠, 옥탄, 노난, 데칸, 클로로벤젠 및 이들의 혼합물로 이루어진 그룹으로부터 선택되는 것임을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 1 항에 있어서,상기 N-치환 말레이미드는 N-페닐 말레이미드인 것을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 1 항에 있어서,상기 실리카 겔은 1~450 메쉬 크기의 것임을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 1 항에 있어서,상기 실리카 겔은 30~60 메쉬 크기의 것임을 특징으로 하는N-치환 말레이미드의 정제방법.
- 삭제
- 제 1 항에 있어서,상기 실리카 겔에 흡착된 N-치환 말레이미드를 용출시키기 위하여 사용되는 상기 비극성 용매의 부피는 상기 실리카 겔 부피의 2배인 것을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 1 항에 있어서,상기 붉은 색의 불순물은 N-치환 말레이미드의 중합 올리고머 또는 그 유사체인 것을 특징으로 하는N-치환 말레이미드의 정제방법.
- 제 1 항에 있어서,상기 실리카 겔 컬럼에 적용되는 상기 N-치환 말레이미드 용액의 온도는 30~50℃인 것을 특징으로 하는N-치환 말레이미드의 정제방법.
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KR1020070104593A KR101051534B1 (ko) | 2007-10-17 | 2007-10-17 | 실리카 겔을 이용한 n-치환 말레이미드의 정제방법 |
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KR1020070104593A KR101051534B1 (ko) | 2007-10-17 | 2007-10-17 | 실리카 겔을 이용한 n-치환 말레이미드의 정제방법 |
Publications (2)
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KR20090039133A KR20090039133A (ko) | 2009-04-22 |
KR101051534B1 true KR101051534B1 (ko) | 2011-07-22 |
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KR1020070104593A KR101051534B1 (ko) | 2007-10-17 | 2007-10-17 | 실리카 겔을 이용한 n-치환 말레이미드의 정제방법 |
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Families Citing this family (2)
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KR102224894B1 (ko) * | 2016-10-05 | 2021-03-05 | 주식회사 엘지화학 | N-치환 말레이미드의 정제 방법 |
KR102111638B1 (ko) * | 2017-12-26 | 2020-05-15 | 주식회사 엘지화학 | N-치환 말레이미드 정제방법 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001302627A (ja) | 2000-04-17 | 2001-10-31 | Nippon Shokubai Co Ltd | N−アルキルマレイミドの精製方法 |
JP2003160557A (ja) | 2001-11-22 | 2003-06-03 | Nippon Shokubai Co Ltd | N−アルキルマレイミドの精製方法およびn−アルキルマレイミド組成物 |
WO2007064306A1 (en) | 2005-11-30 | 2007-06-07 | Vucht, A.S. | Method of preparation of maleimides by thermal cyclization of maleamic acids in th presence of a catalyst |
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- 2007-10-17 KR KR1020070104593A patent/KR101051534B1/ko active IP Right Grant
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001302627A (ja) | 2000-04-17 | 2001-10-31 | Nippon Shokubai Co Ltd | N−アルキルマレイミドの精製方法 |
JP2003160557A (ja) | 2001-11-22 | 2003-06-03 | Nippon Shokubai Co Ltd | N−アルキルマレイミドの精製方法およびn−アルキルマレイミド組成物 |
WO2007064306A1 (en) | 2005-11-30 | 2007-06-07 | Vucht, A.S. | Method of preparation of maleimides by thermal cyclization of maleamic acids in th presence of a catalyst |
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