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1. 发明公开

KR1020030032185A Ｎ,Ｎ'-비스[2,3-디히드록시프로필]-2,4,6-트리요오드-5-아세틸아미도 이소 프탈아미드의 결정화방법 无效
标题翻译： N，N'-二（2,3-二羟基丙基）-2,4,6-三异丙基-5-乙酰氨基乙酰胺的结晶
公开(公告)号：KR1020030032185A
公开(公告)日：2003-04-26
申请号：KR1020010063774
申请日：2001-10-16
申请人： 동국제약 주식회사
发明人： 최경석 , 홍순명 , 이승화 , 신순철 , 송경상 , 박진규 , 차경회 , 임대성 , 이인규 , 백동렬
IPC分类号： C07F13/00
CPC分类号： C07C231/22 , C07C231/14 , C07C235/48
摘要： PURPOSE: Provided is a crystallization method of crude N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-5-acetylamidoisophthalamide in a mixed solvent of water and acetone or methanol and ethanol to obtain N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-5-acetylamidoisophthalamide having high purity of 99.4% in a high yield of 99.9%. CONSTITUTION: The N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-5-acetylamidoisophthalamide is represented by formula(1) and is an intermediate of iohexol which is used as a contrast medium in X-ray picture. Its crystallization method comprises the steps of: preparing a crude solution of N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-5-acetylamidoisophthalamide by using, as starting material, 5-acetamido-2,4,6-triiodoisophthaloyl chloride and 3-amino 1,2-propanediol; concentrating the solvent, dimethylacetamide in the crude solution; adding to the concentrate a mixed solvent consisting of 30-60%(v/v) of water and 40-70%(v/v) of acetone or mixture of 40-60%(v/v) of methanol and 40-60% of ethanol with refluxing to obtain crystals; and cooling the obtained crystals at room temperature then purifying them.
摘要翻译：目的：提供粗N，N'-双（2,3-二羟基丙基）-2,4,6-三碘-5-乙酰氨基间苯二甲酰胺在水和丙酮或甲醇和乙醇的混合溶剂中的结晶方法，得到N，（2,3-二羟基丙基）-2,4,6-三碘-5-乙酰氨基间苯二甲酰胺，高纯度为99.4％，99.9％的高收率。构成：N，N'-双（2,3-二羟基丙基）-2,4,6-三碘-5-乙酰氨基间苯二甲酰胺由式（1）表示，是在X中用作造影剂的碘海醇中间体 -ray图片。其结晶方法包括以下步骤：以N，N'-双（2,3-二羟基丙基）-2,4,6-三碘-5-乙酰氨基间苯二甲酰胺为原料，使用5-乙酰氨基-2 ，4,6-三碘间苯二酰氯和3-氨基1,2-丙二醇; 浓缩溶剂，二甲基乙酰胺在粗溶液中; 向浓缩物中加入由30-60％（v / v）水和40-70％（v / v）丙酮或40-60％（v / v）甲醇和40-60％（v / v）甲醇的混合物组成的混合溶剂％的乙醇回流以获得晶体; 并在室温下冷却所得晶体，然后进行纯化。

2. 发明公开

KR1020000047871A 고순도 2,6-디이소프로필페놀의 정제방법 无效
标题翻译：高纯度2,6-二羟基苯酚的精制方法
公开(公告)号：KR1020000047871A
公开(公告)日：2000-07-25
申请号：KR1019990054574
申请日：1999-12-02
申请人： 동국제약 주식회사
发明人： 박진규 , 최경석
IPC分类号： C07C37/68
摘要： PURPOSE: A refinement method of 2,6-diisopropylphenol(DIP) is provided which enables DIP with high purity to produce for industrial use so that it is possible to produce DIP in an enormous volume. CONSTITUTION: In the refinement method of 2,6-diisopropylphenol(DIP) of formula 1 with not less than 90% purity, it is characterized by using an inorganic acid in a first step and a base in a second step, extracting in an extraction solvent, distilling again or crystallizing at -20 to -30°C to produce DIP. The inorganic acid is one selected from HCl, H2SO4 and H3PO4 and has 1-10N concentration. The base is selected from NaOH, KOH, LiOH, Ca(OH)2, Mg(OH)2 and Al(OH)3 used at 1-10% concentration and is controlled in pH 8-12. The solvent in extraction is selected from oil ether, n-hexane, carbon tetrachloride, chloroform and methylene chloride.
摘要翻译：目的：提供2,6-二异丙基苯酚（DIP）的精制方法，其使得能够生产高纯度的DIP用于工业用途，使得可以大量生产DIP。构成：在具有不低于90％纯度的式1的2,6-二异丙基苯酚（DIP）的精制方法中，其特征在于在第一步中使用无机酸，在第二步中使用碱，在萃取中萃取溶剂，再次蒸馏或在-20至-30℃下结晶以产生DIP。无机酸选自HCl，H2SO4和H3PO4，浓度为1-10N。碱选自NaOH浓度为1-10％的NaOH，KOH，LiOH，Ca（OH）2，Mg（OH）2和Al（OH）3，控制在pH8-12。萃取中的溶剂选自油醚，正己烷，四氯化碳，氯仿和二氯甲烷。

3. 发明公开

KR1020030033386A 이오헥솔의 제조방법 无效
标题翻译：制备IOHEXOL的方法
公开(公告)号：KR1020030033386A
公开(公告)日：2003-05-01
申请号：KR1020010065135
申请日：2001-10-22
申请人： 동국제약 주식회사
发明人： 최경석 , 홍순명 , 이승화 , 신순철 , 송경상 , 박진규 , 차경회 , 임대성 , 이인규 , 백동렬
IPC分类号： C07F13/00
CPC分类号： C07C231/22 , C07C231/12 , C07C235/48
摘要： PURPOSE: Provided is a process for preparing iohexol by using ethanol or dimethylacetamide as a reaction solvent, thereby rapidly and simply preparing the iohexol in higher yield. CONSTITUTION: A process for preparing iohexol of the formula(1) comprises the steps of: dissolving N,N' - bis £2,3 - dihydroxypropyl| - 2,4,6 - triiodine - 5 - acetylamido isophthalamide and lithium hydroxide monohydrate in ethanol or dimethylacetamide; cooling the solution at 0 to 4 deg. C; and adding 3-chloro-1,2-propanediol into the solution and reacting them to crystalize iohexol, wherein lithium hydroxide monohydrate is added in an amount of 0.5 to 2.5 moles per 1 mole of N,N' - bis £2,3 - dihydroxypropyl| - 2,4,6 - triiodine - 5 - acetylamido isophthalamide; the volume of ethanol or dimethylacetamide used is 1.2 to 1.4 times of 1 mole of N,N' - bis £2,3 - dihydroxypropyl| - 2,4,6 - triiodine - 5 - acetylamido isophthalamide; 3-chloro-1,2-propanediol is added in an amount of 0.5 to 2.5 moles per 1 mole of N,N' - bis £2,3 - dihydroxypropyl| - 2,4,6 - triiodine - 5 - acetylamido isophthalamide; and the reaction is carried out at 0 to 60 deg. C for 25 to 37 hours.
摘要翻译：目的：提供通过使用乙醇或二甲基乙酰胺作为反应溶剂制备碘海醇的方法，从而快速且简单地以高产率制备碘海醇。构成：式（1）的碘海醇的制备方法包括以下步骤：将N，N'-二2,3-二羟丙基| -2,4,6-三碘乙酰乙酰氨基间苯二甲酰胺和氢氧化锂一水合物在乙醇或二甲基乙酰胺中; 在0至4度冷却溶液。 C; 并向溶液中加入3-氯-1,2-丙二醇，并使它们与碘海醇结晶反应，其中每1摩尔N，N'-双2,3,3-三氟乙醇加入0.5至2.5摩尔的氢氧化锂一水合物，二羟基| -2,6,6-三碘代-5-乙酰氨基间苯二胺; 使用的乙醇或二甲基乙酰胺的体积为1摩尔N，N'-二2,3-二羟丙基| -2,6,6-三碘代-5-乙酰氨基间苯二胺; 加入3-氯-1,2-丙二醇的量为0.5至2.5摩尔/ 1摩尔N，N'-二2,3-二羟丙基| -2,6,6-三碘代-5-乙酰氨基间苯二胺; 反应在0〜60℃进行。 C为25至37小时。

4. 发明授权

KR100308876B1 옥사졸린 화합물의 제조방법 失效
标题翻译：恶唑啉化合物的制备方法
公开(公告)号：KR100308876B1
公开(公告)日：2001-09-26
申请号：KR1019990000836
申请日：1999-01-14
申请人： 동국제약 주식회사
发明人： 박진규 , 최경석 , 이한원 , 서성기 , 함원훈 , 오창영 , 이기영 , 김용현 , 박민성
IPC分类号： C07D263/02
摘要： 본발명은약리학적활성이강한화합물인베타-아미노-알파-히드록시산또는감마-아미노-베타-히드록시산으로화학적전환이용이한옥사졸린화합물을제조하는방법에관한것이다. 먼저알라닌, 발린, 루이신, 시스테인, 시클로헥실글리신, 시클로헥실알라닌, 페닐글리신, p-히드록시페닐글리신, 페닐알라닌또는 p-히드록시페닐알라닌과같은α-아미노산으로하기구조식 (4)의화합물을제조한후 팔라듐화합물을촉매로분자내고리화반응을이용하여옥사졸린화합물(3)을제조한다. 그런다음옥사졸린화합물(3)의비닐그룹(vinyl group)을 RuCl와 NaIO를이용한산화반응으로베타-아미노-알파-히드록시산으로화학적전환이용이한옥사졸린화합물(1)을합성하거나, 또는옥사졸린화합물(3)의비닐그룹을 9-Borabicyclo[3.3.1]nonane으로말단에히드록시그룹을도입하고말단히드록시그룹을 RuCl와 NaIO를이용한산화반응으로감마-아미노-베타-히드록시산으로화학적전환이용이한옥사졸린화합물(2)을제조할수 있다.

5. 发明公开

KR1020000075115A 불순물 Ｃ가 제거된 이오파미돌의 신규 제조방법 无效
标题翻译：通过去除污染物制备IOPAMIDOL的新方法C
公开(公告)号：KR1020000075115A
公开(公告)日：2000-12-15
申请号：KR1019990019517
申请日：1999-05-28
申请人： 동국제약 주식회사
发明人： 허정호 , 박진규 , 최경석 , 임대성
IPC分类号： C07C233/02
摘要： PURPOSE: A novel method for preparing iopamidol useful as an X-ray contrast medium by controlling a precursor of an impurity C in a synthetic process is provided which produces the iopamidol in a simple manner and in high yields. CONSTITUTION: In the process for manufacturing iopamidol by synthesizing 5-amino-2,4,6-triiodoisophthalic acid dichloride and L-2-acetoxypropionyl chloride, it comprises the steps of adding L-2-acetoxypropionyl chloride to a basic solvent such as N,N-dimethylacetamide dichloride or N,N-dimethylformamide and agitating at ordinary temperatures; and adding 5-amino-2,4,6-triiodoisophthalic acid dichloride thereto.
摘要翻译：目的：提供通过在合成方法中控制杂质C的前体而用作X射线造影剂的碘帕醇的新方法，其以简单的方式和高产率产生碘帕醇。构成：在通过合成5-氨基-2,4,6-三碘代邻苯二甲酸二氯化物和L-2-乙酰氧基丙酰氯制备碘帕醇的方法中，包括将L-2-乙酰氧基丙酰氯加入到碱性溶剂如N ，N-二甲基乙酰胺二氯化物或N，N-二甲基甲酰胺，并在常温下搅拌; 并向其中加入5-氨基-2,4,6-三碘代邻苯二甲酸二氯化物。

6. 发明公开

KR1020000061780A 이오프로마이드의 제조방법 失效
标题翻译：生产眼药水的方法
公开(公告)号：KR1020000061780A
公开(公告)日：2000-10-25
申请号：KR1019990011106
申请日：1999-03-31
申请人： 동국제약 주식회사
发明人： 심상철 , 최흥진 , 이동엽 , 이인규 , 최경석 , 박진규
IPC分类号： C07C233/64 , C07C231/12
摘要： PURPOSE: Provided is iopromide produced from 5-aminoisophthalate, which can be used for X-ray contrast media. CONSTITUTION: The iopromide(formula 1) is produced by a process comprising the steps of: (1) reacting 5-aminoisophthalate with KICl2 in the presence of iodine to obtain 5-amino-2,4,6-triiodoisophthalate; (2) reacting the 5-amino-2,4,6-triiodoisophthalate with the minimum quantity of thionyl chloride in ethyl acetate as a solvent to obtain 5-amino-2,4,6-triiodoisophthalate chloride; (3) reacting the 5-amino-2,4,6-triiodoisophthalate chloride with methoxy acetate in the presence of phosphorous pentachloride to obtain 5-methoxy acetyl amino-2,4,6-triiodoisophthalate chloride; (4) reacting the 5-methoxy acetyl amino-2,4,6-triiodoisophthalate chloride, 2,3-dihydroxy propyl amine and triethylamine as a neutralizing agent of HCl to obtain the iopromide (5-methoxy acetyl amino-2,4,6-triiodoisophthalate diamide).
摘要翻译：目的：提供从5-氨基间苯二甲酸酯生产的碘普罗胺，可用于X射线造影剂。方案：碘普罗胺（式1）通过包括以下步骤的方法制备：（1）在碘存在下使5-氨基间苯二甲酸酯与KICl2反应，得到5-氨基-2,4,6-三碘邻苯二甲酸酯; （2）使5-氨基-2,4,6-三碘间苯二甲酸酯与最少量的亚硫酰氯在乙酸乙酯中作溶剂反应，得到5-氨基-2,4,6-三碘间苯二甲酸氯化物; （3）在五氯化磷存在下使5-氨基-2,4,6-三碘间苯二甲酸氯化物与甲氧基乙酸盐反应，得到5-甲氧基乙酰氨基-2,4,6-三碘间苯二甲酸氯化物; （4）将5-甲氧基乙酰氨基-2,4,6-三碘间苯二甲酸氯化物，2,3-二羟基丙基胺和三乙胺作为HCl的中和剂反应，得到碘普罗胺（5-甲氧基乙酰氨基-2,4， 6-三碘邻苯二甲酸二酰胺）。

7. 发明公开

KR1020000050758A 옥사졸린 화합물의 제조방법 失效
标题翻译：制备氧杂环丁烷化合物的方法
公开(公告)号：KR1020000050758A
公开(公告)日：2000-08-05
申请号：KR1019990000836
申请日：1999-01-14
申请人： 동국제약 주식회사
发明人： 박진규 , 최경석 , 이한원 , 서성기 , 함원훈 , 오창영 , 이기영 , 김용현 , 박민성
IPC分类号： C07D263/02
摘要： PURPOSE: Provided is a method for preparing oxazoline compounds which is easy to be chemically converted into beta-amino-alpha-hydroxy acid or gamma-amino-beta-hydroxy acid which has strong pharmacological activities. The produced compounds can be used in the preparation of physiologically active substance. CONSTITUTION: A method comprises the steps of: preparing a compound of formula(3) by cyclization reaction using as a starting material, the alpha-amino acid of formula(4) such as Alanine, Valine, Leucine, Cystein, Cyclohexylglycine, Cyclohexylalanine, Phenylglycine, etc., in the presence of paladium as a catalyst; reacting the compound of formula(3) with 9-Borabicyclo£3.3.1|nonane dissolved in tetrahydrofuran using a first oxidizing agent; and preparing a compound of formula(2) using a mixture of acetonitrile/carbon tetrachloride /water as a solvent and a second oxidizing agent. In formula(3), R is methyl, isopropyl, sec-butyl, thiomethyl, cyclohexyl, cyclohexylmethyl, phenyl, p-hydroxyphenyl or p-hydroxyphenylmethyl.
摘要翻译：目的：提供易于化学转化为具有强药理活性的β-氨基-α-羟基酸或γ-氨基-β-羟基酸的恶唑啉化合物的方法。生成的化合物可用于制备生理活性物质。构成：一种方法包括以下步骤：通过使用作为起始原料的环化反应制备式（3）的化合物，式（4）的α-氨基酸如丙氨酸，缬氨酸，亮氨酸，半胱氨酸，环己基甘氨酸，环己基丙氨酸，苯基甘氨酸等，在作为催化剂的the存在的情况下，使用第一氧化剂使式（3）化合物与9-硼杂双环{3.3.1 |壬烷溶解在四氢呋喃中; 并使用乙腈/四氯化碳/水作为溶剂和第二氧化剂的混合物制备式（2）的化合物。在式（3）中，R是甲基，异丙基，仲丁基，硫代甲基，环己基，环己基甲基，苯基，对羟基苯基或对羟基苯基甲基。

8. 发明授权

KR100282011B1 고순도 2,6-디이소프로필페놀의 제조방법 失效
标题翻译：生产高纯度2,6-二异丙基苯酚的方法
公开(公告)号：KR100282011B1
公开(公告)日：2001-02-15
申请号：KR1019980016238
申请日：1998-05-07
申请人： 동국제약 주식회사
发明人： 박진규 , 최경석 , 김남진 , 이동준
IPC分类号： C07C39/06
摘要： 본 발명은 순도 95% 이상의 페놀에 나트륨, 칼륨, 마그네슘, 알루미늄, 망간, 철에서 선택된 1종이상의 금속 화합물을 첨가하고, 반응액 중량대비 0.1∼1.0%의 유기산 또는 무기산을 가하여 액상을 산성화시킨 후, 프로필렌가스를 300∼700psi의 고압으로 주입하여 200∼300℃의 고온, 250∼450psi의 고압하에서 선택적으로 2,6-디이소프로필페놀을 합성하고, 진공 증류를 통하여 99.8%이상의 고순도로 2,6-디이소프로필페놀을 제조하는 방법에 관한 것이다.

9. 发明公开

KR1020000031642A 이오파미돌의 결정화 방법 无效
标题翻译： IOPAMIDOL的结晶方法
公开(公告)号：KR1020000031642A
公开(公告)日：2000-06-05
申请号：KR1019980047785
申请日：1998-11-09
申请人： 동국제약 주식회사
发明人： 박진규 , 최경석 , 이동엽 , 이인규 , 송창헌 , 이동준
IPC分类号： C07C231/22
CPC分类号： C07C231/24 , C07C237/46
摘要： PURPOSE: Iopamidol having a pure anhydrous compound for X-ray contrast medium without a hydrate 1 and a hydrate 5 is provided by using a solvent having mixed water and alcohol. Thereby, it is possible to obtain iopamidol having a pure anhydrous compound with purity of at least 99.5% and yield of at least 90%, so that mass production is possible. CONSTITUTION: The method for crystallization of iopamidol contains following the steps of: solving an iopamidol in the vaporized water to vaporize the water; removing the vaporized water to add an alcohol; and then refluxing the mixture for 3-4hour to obtain the iopamidol of white crystal. A ratio of iopamidol to vaporized water is 10: 1(w/v) to 1: 1(w/v) and a ratio of iopamidol to alcohol is 1: 1(w/v) to 1: 10(w/v). The alcohol is consisted of ethanol and propanol. A ratio of iopamidol: water: ethanol is 4: 1: 8(w/v/v). When the reflux time is 4hour, anhydrous iopamidol having solubility of at least 80% is obtained.
摘要翻译：目的：通过使用具有混合水和醇的溶剂，提供具有无水合物1和水合物5的X射线造影剂的纯无水化合物的Iopamidol。由此，可以得到纯度至少为99.5％，产率至少为90％的纯无水化合物的碘帕醇，可以批量生产。结论：碘帕醇的结晶方法包括以下步骤：在汽化水中溶解碘帕醇以蒸发水; 除去蒸发的水加入酒精; 然后将混合物回流3-4小时，得到白色结晶的碘帕醇。碘帕醇与汽化水的比例为10：1（w / v）至1：1（w / v），碘帕醇与酒精的比例为1:1（w / v）至1:10（w / v）。酒精由乙醇和丙醇组成。碘帕醇：水：乙醇的比例为4：1：8（w / v / v）。当回流时间为4小时时，获得具有至少80％的溶解度的无水碘帕醇。

10. 发明公开

KR1020030032184A 이오헥솔의 결정화방법 无效
标题翻译： IOHEXOL的结晶方法
公开(公告)号：KR1020030032184A
公开(公告)日：2003-04-26
申请号：KR1020010063773
申请日：2001-10-16
申请人： 동국제약 주식회사
发明人： 최경석 , 홍순명 , 이승화 , 신순철 , 송경상 , 박진규 , 차경회 , 임대성 , 이인규 , 백동렬
IPC分类号： C07C231/24
摘要： PURPOSE: A crystallization method of iohexol is provided to obtain the iohexol of high purity in a high production yield from the unpurified iohexol by using a mixture solvent of methanol and ethanol without using a crystal seed. CONSTITUTION: The crystallization method comprises the steps of adding methanol to the unpurified iohexol to dissolve iohexol into methanol, and decolorizing the solution and removing the impurities from the solution by using an adsorbent; and concentrating the methanol solution, adding ethanol to the solution and refluxing the obtained solvent mixture. Preferably, the absorbent is active carbon; and the solvent mixture comprises 1-20 vol% of methanol and 80-99 vol% of ethanol.
摘要翻译：目的：提供碘海醇的结晶方法，通过使用不使用晶种的甲醇和乙醇的混合溶剂，从未纯化的碘海醇中获得高产率的高纯度碘海醇。结论：结晶方法包括将甲醇加入到未纯化的碘海醇中以将碘海醇溶解在甲醇中，并使用吸附剂将溶液脱色并从溶液中除去杂质的步骤; 并浓缩甲醇溶液，向溶液中加入乙醇并回流得到的溶剂混合物。优选地，吸收剂是活性炭; 溶剂混合物含有1-20体积％的甲醇和80-99体积％的乙醇。

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