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12.发明公开이미다졸리움염에 고정화된 오스뮴 촉매와 키랄 리간드를 이용한 이웃한 키랄 다이올 화합물의 제조 방법 및 촉매회수 방법 失效通过使用固定在咪达拉斯钠盐和乳酸配位体上的硅酸盐催化剂来制备维生素二醇化合物的方法，以改善生产能力并易于回收所用的催化剂，具有经济有利的作用
公开(公告)号：KR1020040090283A
公开(公告)日：2004-10-22
申请号：KR1020030024334
申请日：2003-04-17
Applicant: 한국과학기술연구원
IPC: C07C29/74
CPC classification number: Y02P20/584
Abstract: PURPOSE: A method for preparing vicinal chiral diol compounds through asymmetric dehydroxylation by using an osmium catalyst immobilized to imidazolium salts and chiral ligands, is provided to improve the production yield with high optical purity and recycling properties, without deteriorating the catalyst activity and enantiomeric excess. The method is environmentally friendly, due to the immobilization of the highly toxic and volatile osmium compound. CONSTITUTION: The method for preparing neighboring chiral diol compounds by using an osmium catalyst immobilized to imidazolium salts comprises: (1) adding chiral ligands represented by formulas 1 and 2, an imidazolium salt represented by formula 3 and an osmium catalyst to a solvent with stirring, and then further adding an auxiliary oxidizer and olefin compounds thereto with stirring; (2) removing all of the volatile compounds under reduced pressure; (3) extracting the residues free of volatile compounds from the step (2) with an organic solvent; and (4) separating vicinal chiral diol compounds out of the organic phase of the step (3).
Abstract translation: 目的：提供通过使用固定在咪唑鎓盐和手性配体上的锇催化剂通过不对称脱羟基化制备邻位手性二醇化合物的方法，以提高具有高光学纯度和再循环性能的产率，而不会降低催化剂活性和对映体过量。 该方法是环境友好的，由于高毒性和挥发性锇化合物的固定。 构成：通过使用固定在咪唑鎓盐上的锇催化剂制备相邻的手性二醇化合物的方法包括：（1）将由式1和2表示的手性配体，式3表示的咪唑盐和锇催化剂加入到溶剂中，同时搅拌 ，然后在搅拌下进一步加入辅助氧化剂和烯烃化合物; （2）减压除去所有的挥发性化合物; （3）用有机溶剂从步骤（2）中提取不含挥发性化合物的残留物; 和（4）从步骤（3）的有机相中分离出相邻的手性二醇化合物。
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公开(公告)号：KR1020020009277A
公开(公告)日：2002-02-01
申请号：KR1020000042858
申请日：2000-07-25
Applicant: 한국과학기술연구원 , 한화화인케미칼 주식회사
IPC: C07C251/24
Abstract: PURPOSE: Provided are a chiral salen derivative used as a chiral ligand in an asymmetric epoxidation of olefin for producing chiral epoxy compounds and a chiral salen-metal derivative used as a chiral catalyst in the asymmetric epoxidation of olefin. CONSTITUTION: The chiral salen derivative is represented by the formula 1 and the chiral salen-metal derivative is represented by the formula 3, wherein R is C1-C24 straight or branched alkyl, halogen, alcohol, mercapto, or carboxyl-substituted C1-C24 straight or branched alkyl, cycloalkyl, aryl, or heteroaryl, H(1) and H(2) are trans each other, M is a transition metal ion such as Cr, Mn, V, Fe, Mo, W, Ru, Co, Ti, or Os, and A is an anion such as Cl-, CH3COO-, PF6-, or SbF6-.
Abstract translation: 目的：提供用作生产手性环氧化合物的烯烃不对称环氧化的手性配体的手性色胺衍生物和在烯烃的不对称环氧化中用作手性催化剂的手性盐金属衍生物。 构成：手性盐酸衍生物由式1表示，手性盐金属衍生物由式3表示，其中R为C1-C24直链或支链烷基，卤素，醇，巯基或羧基取代的C1-C24 直链或支链烷基，环烷基，芳基或杂芳基，H（1）和H（2）彼此相互反转，M是过渡金属离子如Cr，Mn，V，Fe，Mo，W，Ru，Co， Ti或Os，A是阴离子如Cl-，CH 3 COO-，PF 6 - 或SbF 6 - 。
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公开(公告)号：KR1020010060120A
公开(公告)日：2001-07-06
申请号：KR1019990068242
申请日：1999-12-31
Applicant: 한국과학기술연구원 , 한화화인케미칼 주식회사
IPC: C07C51/00
Abstract: PURPOSE: A method for preparing ethyl (R)-2-bromo-4-phenylbutyrate and intermediates for preparing the compound are provided, which compound is useful as the intermediate for the preparation of antihypertensive. CONSTITUTION: The intermediates for preparing ethyl (R)-2-bromo-4-phenylbutyrate represented by the formula 1 is the oxazolidinone derivatives of 4-phenylbutyric acid represented by the formula 2, and the oxazolidinone derivatives of (2R)-2-bromo-4-phenylbutyric acid represented by the formula 3. The method comprises the steps of reacting 4-phenylburyric acid and the oxazolidinone of the formula 5 to obtain the compound of the formula 2; reacting the compound of the formula 2 and a bromization agent to obtain the compound of the formula 3; and reacting the compound of the formula 3 and a nucleophilic ethoxide to obtain the compound of the formula 1. Preferably the bromization agent is N-bromosuccinimide or bromine; and the ethoxide is lithium ethoxide, sodium ethoxide, magnesium ethoxide or titanium ethoxide. In the formulas 1, 2, 3 and 5, R1 is a methyl group and R2 is a phenyl group, or R1 is a phenyl group and R2 is H.
Abstract translation: 目的：提供（R）-2-溴-4-苯基丁酸乙酯的制备方法和制备该化合物的中间体，该化合物可用作制备抗高血压药物的中间体。 构成：由式1表示的（R）-2-溴-4-苯基丁酸乙酯的中间体是由式2表示的4-苯基丁酸的恶唑烷酮衍生物，（2R）-2-溴的恶唑烷酮衍生物 -4-苯基丁酸。该方法包括使4-苯基丙酸与式5的恶唑烷酮反应得到式2化合物的步骤; 使式2的化合物与溴化剂反应得到式3的化合物; 并使式3化合物与亲核乙醇盐反应，得到式1的化合物。优选溴化剂为N-溴代琥珀酰亚胺或溴; 乙醇钠是乙醇锂，乙醇钠，乙醇镁或乙醇钛。 在式1，2，3和5中，R 1是甲基，R 2是苯基，或者R 1是苯基，R 2是H.
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公开(公告)号：KR1019950011929B1
公开(公告)日：1995-10-12
申请号：KR1019920017280
申请日：1992-09-22
Applicant: 한국과학기술연구원
IPC: B01J20/20
Abstract: (A) adding inorganic acid or alkali to carbonized rice bran or silver white rice bran, followed by heat refluxing ; (B) cooling down the rice bran to room temperature, followed by neutralizing and washing with water ; and (C) filtering and drying the rice bran so that dissolved silicate in rice bran is removed. Inorganic acid is selected from hydrochloric acid, nitric acid and fluoric acid. Alkali is selected from sodium hydroxide and potassium hydroxide. Waste water is purified by contacting with the prepared rice bran to remove hazardous contaminants dissolved in the water.
Abstract translation: （A）向碳化米糠或银白米糠中加入无机酸或碱，然后加热回流; （B）将米糠冷却至室温，然后用水中和和洗涤; 和（C）过滤并干燥米糠，使米糠中溶解的硅酸盐被去除。 无机酸选自盐酸，硝酸和氟酸。 碱选自氢氧化钠和氢氧化钾。 废水通过与制备的米糠接触来净化，以除去溶解在水中的有害污染物。
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Patent Agency Ranking
公开(公告)号：KR1019950014124A
公开(公告)日：1995-06-15
申请号：KR1019930023899
申请日：1993-11-11
Applicant: 한국과학기술연구원
IPC: C07D501/59
Abstract: 본 발명은 소위 세파클로르도 불리우는 7-(D-아미노-2-페닐아세트아미도)-3-클로로-3-세펨-4-카르복실산의 제조에 유용한 중간체들을 제조하기 위한 신규 고 개략된 방법을 제공한다. 본 발명의 방법은 디페닐메틸 7-페닐아세트아미도-3-히드록시-3-세펨-4-카르복실레이트 화합물(XI)이나 이의 톨루엔 1:1 용매화합물을 디메틸포름아미드내에서 0.5-2당량의 삼염화인, 1-3당량의 포스포 릴클로라이드, 1.5-3.5당량의 포스겐 및 1.5-3.5 당량의 옥살릴클로라이드에서 선택된 염소화제와 반응시켜 디패닐메틸 7-페닐아세트아미도-3-클로로-3-세펨-4-카르복실레이트 화합물(Ⅱ)을 제조 하는 제1공정; 제1공정에서 얻은 디페닐메틸 7-페닐아세트아미도-3-클로로-3-세펨-4-카르복실 레이트 화합물(Ⅱ)을 디플로로메탄, 1, 2-디클로로에탄 및 데트라히드로푸란에서 선택된 비활성 유기 용매내에서 1.6-3당랑의 오염화인 및 2-3당량의 피리딘과 반옹시킨 뒤 여기에 C
l -C
12 의 지방족 알코올을 가하여 반응시켜 디페닐메틸 7-아미노-3-클로로-3-세펨-4-카르복실레이트 화합물(Ⅲ)을 제조하는 제2공정; 및 제2공정에서 얻은 디페닐메틸 7-아미노-3-클로로-3-세펨-4-카르복실레이트 화합물(Ⅳ)을 개미산 혹은 페놀과 반응시켜 7-아미노-3-클로로-3-세펨-4-카르복실레이트 화합물(Ⅳ)을 제조하는 제3공정으로 이루어지는 것을 특징으로 한다.-
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公开(公告)号：KR1020040004862A
公开(公告)日：2004-01-16
申请号：KR1020020038929
申请日：2002-07-05
Applicant: 한국과학기술연구원
IPC: B01J20/02
CPC classification number: B01J31/06 , B01J35/023 , B01J35/1004 , B01J35/1052 , B01J37/0009 , C07C29/00
Abstract: PURPOSE: Provided are osmium tetroxide fixed onto porous adsorbent of nonionic polymer wherein the osmium tetroxide has low toxicity, and high activity and selectivity, the osmium tetroxide being capable of being recovered by a normal filtration and being reused, and further being capable of producing diols with high purity with high efficiency by being used as catalyst in a dihydroxylation process, a method for preparing the same and its use. CONSTITUTION: The osmium tetroxide-adsorbent complex comprises osmium tetroxide fixed onto porous nonionic polymer adsorbent which is a copolymer containing styrene, divinylbenzene, acrylate, or methacrylate monomer, has a pore with 50 to 1000Å and is 20 to 200 μm, wherein the surface area of the polymer is 200 to 1500 m¬2/g. The method comprises the steps of (a) dispersing porous nonionic polymer adsorbent into solvent, and (b) adding osmium tetroxide into the solution obtained at the step (a) so as to cause reaction between the adsorbent and osmium tetroxide, wherein the solvent is water, C1-C4 alcohol or its mixture solution and the reaction of the step (b) is performed at 0 to 60°C for 2 to 6 hrs. The osmium tetroxide is used as a catalyst in asymmetric dihydroxylation, thereby producing diols.
Abstract translation: 目的：提供四氧化锇固定在非离子聚合物的多孔吸附剂上，其中四氧化锇具有低毒性，高活性和选择性，四氧化锇能够通过正常过滤回收并再次使用，并且还能够生产二醇 通过在二羟基化方法中用作催化剂，其高纯度，高效率，其制备方法及其用途。 构成：四氧化锇 - 吸附剂络合物包括固定在多孔非离子聚合物吸附剂上的四氧化锇，其是含有苯乙烯，二乙烯基苯，丙烯酸酯或甲基丙烯酸酯单体的共聚物，具有50至1000埃的孔，为20至200微米，其中表面积 的聚合物为200〜1500m2 / g。 该方法包括以下步骤：（a）将多孔非离子聚合物吸附剂分散在溶剂中，（b）在步骤（a）中得到的溶液中加入四氧化锇，以使吸附剂与四氧化锇之间发生反应，其中溶剂为 水，C1-C4醇或其混合溶液，并且步骤（b）的反应在0至60℃下进行2至6小时。 四氧化锇用作不对称二羟基化反应中的催化剂，从而产生二醇。
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公开(公告)号：KR100404587B1
公开(公告)日：2003-11-05
申请号：KR1020010011600
申请日：2001-03-07
Applicant: 한국과학기술연구원
IPC: C07D301/03
Abstract: 본 발명은 키랄 에폭사이드를 제조하는 방법에 관한 것으로서, 구체적으로 이온성 액체 용매에서 키랄 살렌금속촉매 존재하에 올레핀과 산화제를 반응시켜 비대칭 에폭시화 반응에 의해 키랄 에폭사이드를 제조하는 방법에 관한 것으로, 본 발명의 제조방법에 의하면 반응 후 고가의 키랄 살렌금속촉매의 회수를 용이하게 하여 반복적으로 사용할 수 있으므로 경제적으로 키랄 에폭사이드를 제조할 수 있다.
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公开(公告)号：KR100392710B1
公开(公告)日：2003-07-28
申请号：KR1020010015739
申请日：2001-03-26
Applicant: 한국과학기술연구원
IPC: C07C247/04 , C07D211/00 , C07D231/00
Abstract: PURPOSE: Provided is a process for producing a chiral compound by using an enantioselective ring-opening reaction of epoxides in the presence of a chiral salen metal catalyst, which can recover or reuse the chiral salen metal catalyst. CONSTITUTION: The chiral compound is produced by using the enantioselective ring-opening reaction of epoxides in the presence of a salt represented by the formula 1 and the chiral salen metal catalyst represented by the formula 3. In the formula 1, when X is nitrogen, Z is -C(R5)-, R1 and R2 are each C1-C18 alkyl, R3-R5 are each hydrogen or C1-C18 alkyl and when X is carbon, Z is -C(R5)-C(R6)-, R1 is C1-C18 alkyl, R2-R6 are each hydrogen or C1-C18 alkyl, n is an integer of 1-3, and Y- is an anion capable of forming a salt. In the formula 3, R1-R4 are independently hydrogen, alkyl, carboxyl, aryl, and substituted aryl, X1-X8 are independently hydrogen, halogen, alkyl, silyl, silyloxy, alkenyl, and etc., Y1 and Y2 are each hydrogen and alkyl, M is a metal, and A is an anion.
Abstract translation: 目的：提供一种在手性salen金属催化剂存在下使用环氧化物的对映选择性开环反应生产手性化合物的方法，该催化剂可以回收或再利用手性salen金属催化剂。 构成：手性化合物是通过在式1所示的盐和式3所示的手性salen金属催化剂存在下使用环氧化物的对映选择性开环反应而制备的。在式1中，当X是氮时， Z为-C（R 5） - ，R 1和R 2各自为C 1 -C 18烷基，R 3 -R 5各自为氢或C 1 -C 18烷基，并且当X为碳时，Z为-C（R 5）-C（R 6） - ， R1是C1-C18烷基，R2-R6各自是氢或C1-C18烷基，n是1-3的整数，Y-是能形成盐的阴离子。 在式3中，R 1 -R 4独立地为氢，烷基，羧基，芳基和取代的芳基，X 1 -X 8独立地为氢，卤素，烷基，甲硅烷基，甲硅烷氧基和链烯基等，Y 1和Y 2各自为氢， 烷基，M是金属，A是阴离子。
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