公开(公告)号：KR1020030073450A

公开(公告)日：2003-09-19

申请号：KR1020020013013

申请日：2002-03-11

Applicant: 화일약품주식회사

Inventor： 양민승 ,  이영남 ,  강병규

IPC: C07C231/00

Abstract: PURPOSE: Provided is an industrially available method for producing 2-hydroxy-N-(2-hydroxyethyl)-3- methoxy-5-(2-propenyl)benzamide in substantially higher yield than that of existing method. CONSTITUTION: The method comprises the steps of (i) reacting a compound of formula II with allyl bromide in the presence of alkali to form a compound of formula III; (ii) performing a Claisen rearrangement of the compound of formula III with heating, so as to form a compound of formula IV; and (iii) reacting the compound of formula IV with ethanolamine to form a compound of formula V. In the formulas, R is C1-C9 alkyl group, provided that ethyl group is excluded.

Abstract translation: 目的：提供了一种以比现有方法更高的产率生产2-羟基-N-（2-羟乙基）-3-甲氧基-5-（2-丙烯基）苯甲酰胺的工业上可用的方法。 方法：该方法包括以下步骤：（ⅰ）在碱的存在下使式Ⅱ化合物与烯丙基溴反应，形成式Ⅲ化合物; （ii）通过加热进行式III化合物的Claisen重排，以形成式IV的化合物; 和（iii）使式IV化合物与乙醇胺反应以形成式V化合物。在式中，R是C1-C9烷基，条件是排除乙基。

公开(公告)号：KR100989389B1

公开(公告)日：2010-10-25

申请号：KR1020100056668

申请日：2010-06-15

Applicant: 화일약품주식회사

Inventor： 정용호 ,  정춘원 ,  이중우 ,  이윤승 ,  김경철 ,  강병규

IPC: C07D417/04 ,  C07D403/06 ,  A61K31/497 ,  A61P25/18

Abstract: PURPOSE: A ziprasidone hydrochloride 1.5 hydrate with novel crystal and a method for preparing the same are provided to ensure 99.5% or more of crystal purity and high stability. CONSTITUTION: A method for preparing crystalline ziprasidone hydrochloride 1.5 hydrate comprises: a step of recrystalizing ziprasidone base in a solvent containing 1-methyl-2-pyrrolidone or dimethylsulfoxide; a step of adding t-butylmethyl ether, buthylmethyl ether and sec-butylmethyl ether or mixture thereof to prepare slurry; and a step of obtaining crystalline ziprasidone hydrochloride 1.5 hydrate.

Abstract translation: 目的：提供具有新晶体的齐拉西酮盐酸盐1.5水合物及其制备方法，以确保99.5％以上的晶体纯度和高稳定性。 结构：制备结晶齐拉昔酮盐酸盐1.5水合物的方法包括：在含1-甲基-2-吡咯烷酮或二甲基亚砜的溶剂中重结晶齐拉西酮碱的步骤; 加入叔丁基甲基醚，丁基甲基醚和仲丁基甲基醚或其混合物以制备浆料的步骤; 和获得结晶的齐拉昔酮盐酸盐1.5水合物的步骤。

公开(公告)号：KR1020100063915A

公开(公告)日：2010-06-14

申请号：KR1020080122284

申请日：2008-12-04

Applicant: 화일약품주식회사

Inventor： 정용호 ,  강병규 ,  이중우

IPC: C07D211/90

Abstract: PURPOSE: A method for isolating and preparing S-(-)-amlodipine is provided to simply and economically isolate and prepare S-(-)-amlodipine having high optical purity. CONSTITUTION: A method for preparing S-(-)-amlodipine compound of chemical formula 1 comprises: a step of reacting racemic amlodipine with L-tartaric acid in tetrahydrofuran solvent; a step of isolating the reactant to precipitate and reaction solution; a step of reacting the isolated reaction solution with D-tartaric acid; a step of reacting (S)-(-)-amlodipine-hemi-D-tartrate-2THF with reaction solution; and a step of reacting the precipitate and base. The solvent containing tetrahydrofuran is tetrahydrofuran single solvent.

Abstract translation: 目的：分离和制备S - （ - ） - 氨氯地平的方法是简单且经济地分离和制备具有高光学纯度的S - （ - ） - 氨氯地平。 构成：制备化学式1的S - （ - ） - 氨氯地平化合物的方法包括：将外消旋氨氯地平与L-酒石酸在四氢呋喃溶剂中反应的步骤; 分离反应物沉淀和反应溶液的步骤; 使分离的反应溶液与D-酒石酸反应的步骤; （S） - （ - ） - 氨氯地平 - 半酒石酸盐-2THF与反应溶液反应的步骤; 和使沉淀物和碱反应的步骤。 含四氢呋喃的溶剂为四氢呋喃单溶剂。

公开(公告)号：KR1020040049044A

公开(公告)日：2004-06-11

申请号：KR1020020076216

申请日：2002-12-03

Applicant: 화일약품주식회사

Inventor： 양민승 ,  이영남 ,  강병규 ,  손옥재

IPC: C07C217/14

Abstract: PURPOSE: Provided is a method of preparing 1,2,3-tris(2-diethylaminoethoxy)benzene and a method of preparing 1,2,3-tris(2-triethylammoniumethoxy)benzene triiodide, gallamine triethiodide. The process enables industrial mass production with high yield. CONSTITUTION: The method of preparing 1,2,3-tris(2-diethylaminoethoxy)benzene comprises the steps of: (a) making pyrogallol lithium salt by reacting pyrogallol and lithium hydroxide or hydrate thereof; and (b) reacting pyrogallol lithium salt obtained from (a) with diethylaminoethyl chloride at 80-130deg.C. The gallamine triethiodide is obtained by reacting 1,2,3-tris(2-diethylaminoethoxy)benzene obtained from (b) with ethyl iodide. The reaction step of (a) and (b) is one pot reaction and the solvent used is selected from acetone, DMF, dioxane, dimethylsulfoxide, acetonitrile, diglyme or their mixture.

Abstract translation: 目的：提供制备1,2,3-三（2-二乙基氨基乙氧基）苯的方法和制备1,2,3-三（2-三乙基铵乙氧基）苯三碘化物，三乙胺三胺盐的方法。 该工艺可以实现大批量生产。 构成：制备1,2,3-三（2-二乙基氨基乙氧基）苯的方法包括以下步骤：（a）通过将连苯三酚和氢氧化锂或其水合物反应制备连苯三酚锂盐; 和（b）将得自（a）的二苯甲基锂盐与二乙基氨基乙基氯在80-130℃反应。 通过使从（b）获得的1,2,3-三（2-二乙基氨基乙氧基）苯与乙基碘反应，得到三乙胺三乙胺。 （a）和（b）的反应步骤是一锅反应，所用溶剂选自丙酮，DMF，二恶烷，二甲亚砜，乙腈，二甘醇二甲醚或其混合物。

公开(公告)号：KR1020040054203A

公开(公告)日：2004-06-25

申请号：KR1020020081025

申请日：2002-12-18

Applicant: 화일약품주식회사

Inventor： 양민승 ,  이영남 ,  강병규 ,  손옥재

IPC: C07D333/36

Abstract: PURPOSE: A process for preparing erdosteine is provided, thereby minimizing formation of impurities and preparing erdosteine in higher yield under mild condition. CONSTITUTION: The process for preparing erdosteine comprises reacting 3-chloroacetamido-2-oxo-tetrahydrothiophene with mercaptoacetic acid in the presence of base and organic solvent or a mixed solvent of organic solvent and water at 45 to 70 deg. C, wherein the base is selected from sodium carbonate, pyridine, ammonia water, diethylamine, triethylamine, 2,6-lutidine, 2,3-lutidine, 3,4-lutidine, lithium hydroxide or hydrates thereof, calcium hydroxide, potassium carbonate, potassium bicarbonate, potassium acetic acid and sodium acetic acid; and the organic solvent is selected from acetone, acetonitrile, N,N-dimethylformamide, 1,4-dioxane, dimethylsulfoxide, ethanol, methanol, tetrahydrofuran or a mixture thereof.

Abstract translation: 目的：提供制备厄多司坦的方法，从而最小化杂质的形成，并在温和条件下以更高的产率制备厄多糖。 构成：制备厄多司坦的方法包括在碱和有机溶剂或有机溶剂和水的混合溶剂的存在下，在45至70℃下使3-氯乙酰氨基-2-氧代 - 四氢噻吩与巯基乙酸反应。 C，其中碱选自碳酸钠，吡啶，氨水，二乙胺，三乙胺，2,6-二甲基吡啶，2,3-二甲基吡啶，3,4-二甲基吡啶，氢氧化锂或其水合物，氢氧化钙，碳酸钾， 碳酸氢钾，乙酸钾和乙酸钠; 有机溶剂选自丙酮，乙腈，N，N-二甲基甲酰胺，1,4-二恶烷，二甲基亚砜，乙醇，甲醇，四氢呋喃或其混合物。

公开(公告)号：KR1020040027045A

公开(公告)日：2004-04-01

申请号：KR1020020058761

申请日：2002-09-27

Applicant: 화일약품주식회사

Inventor： 양민승 ,  이영남 ,  강병규 ,  염을균 ,  이철위 ,  홍기범

IPC: C07D487/04

Abstract: PURPOSE: A process for producing aromatic cyclic derivatives using palladium-loaded zeolite is provided, thereby simplifying the production process of aromatic cyclic derivatives and reducing the production costs by reuse of palladium as catalyst. CONSTITUTION: A process for producing aromatic cyclic derivatives of the formula(1) using palladium-loaded zeolite comprises reacting a compound of the formula(2) or N-acetylated derivatives thereof with a compound of the formula(3) in the presence of chlorine-containing salt and base using palladium-loaded zeolite as catalyst, wherein X is carbohydrate radical and forms aromatic ring with carbon; the aromatic ring comprises one or more hetero selected from N, S and O and is substituted by C1-C4 alkyl, C1-C4 alkoxy or pyrolidinyl; R1 and R2 are independently hydrogen, C1-C18 alkyl, C1-C18 alkoxy - C1-C18 alkyl, C3-C18 cycloalkenyl, phenyl, C1-C4 alkyl and/or halogen substituted phenyl, benzyl, (tetrahydro-pyran-2-yl) oxy-C1-C18 alkyl, (4-methylphenyl)sulfonyl, thiophenyl optionally substituted with acetyl, quinolinyl, pyridinyl optionally substituted with C1-C18 alkyl, tri-C1-C18 alkyl-silyl, or 4,5-dihydro-thiopenyl optionally substituted with acetyl; and Y is halogen.

Abstract translation: 目的：提供使用负载钯的沸石制备芳族环状衍生物的方法，从而简化芳族环状衍生物的制备方法，并通过重新使用钯作为催化剂降低生产成本。 构成：使用负载钯的沸石制备式（1）的芳族环状衍生物的方法包括使式（2）化合物或其N-乙酰化衍生物与式（3）化合物在氯存在下反应 使用负载钯的沸石作为催化剂的盐和碱，其中X是碳水化合物自由基并与碳形成芳环; 芳环包含一个或多个选自N，S和O的杂原子，并被C 1 -C 4烷基，C 1 -C 4烷氧基或吡咯烷基取代; R1和R2独立地是氢，C1-C18烷基，C1-C18烷氧基-C1-C18烷基，C3-C18环烯基，苯基，C1-C4烷基和/或卤素取代的苯基，苄基，（四氢 - 吡喃-2-基 ）氧基-C 1 -C 18烷基，（4-甲基苯基）磺酰基，任选被乙酰基，喹啉基，任选被C 1 -C 18烷基取代的吡啶基，三-C 1 -C 18烷基 - 甲硅烷基或4,5-二氢 - 用乙酰基取代; Y为卤素。

公开(公告)号：KR101125123B1

公开(公告)日：2012-03-16

申请号：KR1020080122284

申请日：2008-12-04

Applicant: 화일약품주식회사

Inventor： 정용호 ,  강병규 ,  이중우

IPC: C07D211/90

Abstract: 본 발명은 테트라히드로푸란(THF) 단독 또는 혼합용매 내에서 L-타르타르산과 D-타르타르산을 사용하여 라세믹 암로디핀으로부터 광학적 이성질체인 S-(-)-암로디핀을 분리 제조하는 방법에 관한 것이다.
암로디핀, 광학분할, 테트라히드로푸란