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1. 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。

2. 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。

3. 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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