公开(公告)号：KR101061256B1

公开(公告)日：2011-08-31

申请号：KR1020090031068

申请日：2009-04-10

Applicant: 한국과학기술연구원

Inventor： 오창현 ,  유병용 ,  김정훈 ,  유승원 ,  구대호

IPC: C07D501/22 ,  C07D501/20 ,  C07D501/06 ,  C07D501/32

CPC classification number: Y02P20/55

Abstract: 본 발명은 새로운 결정형을 갖는 7-아미노-3-비닐-세팔로스포린산염 수화물 및 이의 제조방법에 관한 것으로, 구체적으로 Cu 타겟 방사의 X선 회절 패턴에서, 2θ로 표시된 특성피크가 8.98±0.3, 18.06±0.3, 28.95±0.3, 32.32±0.3, 33.76±0.3 및 34.40±0.3에서 나타나는 새로운 결정형태를 갖는 7-아미노-3-비닐-세팔로스포린산염 수화물 및 이의 제조방법에 관한 것이다. 본 발명에 의하면, 아미노기 보호기의 탈보호화 단계에서 취급이 용이하고 안정한 신타 CLEC-PA(Cross-Linked Enzyme Crystal-Penicilline G Amidase/Acylase) 효소를 이용하여 고순도, 고효율의 새로운 결정성 7-AVCA 수화물을 공업적으로 합성할 수 있어, 상기 7-AVCA를 중간체로 사용하는 세팔로스포린계 항생제 개발시 유용하게 사용될 수 있다.
7-AVCA, 7-아미노-3-비닐-세팔로스포린산, 결정성 수화물, 신타 CLEC-PA 효소, 세파디니르

Abstract translation: 本发明是7-氨基-3-乙烯基具有新晶形 - 涉及头孢菌素盐水合物和其制造方法，特别是在Cu辐射靶的X射线衍射图案，由2θ8.98＆plusmn表示特征峰; 0.3 它们的头孢盐水合物和生产方法 - 7-氨基-3-乙烯基一种具有新晶体形式可出现在0.3 ;, 18.06＆plusmn; 0.3，28.95＆plusmn; 0.3，32.32＆plusmn; 0.3，33.76＆plusmn; 0.3和34.40＆plusmn 它涉及。 根据本发明，容易在氨基保护基团和稳定合酶CLEC-PA（交联酶晶体，青霉素酰化酶/酰化酶）高纯度，高效率的新晶体的脱保护步骤使用酶促7- AVCA水合物处理 可以在工业规模上合成，7-AVCA一个可以有效地头孢菌素用作中间体开发抗生素时使用。

公开(公告)号：KR1020100112672A

公开(公告)日：2010-10-20

申请号：KR1020090031068

申请日：2009-04-10

Applicant: 한국과학기술연구원

Inventor： 오창현 ,  유병용 ,  김정훈 ,  유승원 ,  구대호

IPC: C07D501/22 ,  C07D501/20 ,  C07D501/06 ,  C07D501/32

CPC classification number: Y02P20/55 ,  C07D501/22 ,  A61K31/545

Abstract: PURPOSE: A 7-amino-3-vinyl-cephalosphorinic acid salt hydrate with a novel crystal and a method for preparing the same are provided to industrially synthesize novel crystalline 7-AVCA hydrate of high yield and high purity. CONSTITUTION: A 7-amino-3-vinyl-cephalosphorinic acid salt hydrate of chemical formula 1 with a novel crystal has characteristic peak at 8.98±0.3, 18.06±0.3, 28.95±0.3, 32.32±0.3, 33.76±0.3 and 34.40±0.3. A method for preparing the crystalline 7-amino-3-vinyl-cephalosphorinic acid salt hydrate comprises: a step of adding cresol or phenol to p-methoxybenzyl-7-phenylaceteamido3-vinyl-3-cefem-4-carboxylate and stirring to deprotect a protection group of carboxylic group; a step of adjusting pH with alkali and adding cinta CELC-PA enzyme to deprotect a protection group of amino group; a step of crystallizing the deprotected 7-AVCA by adjusting pH with inorganic acid; and a step of adding methanol solution and base to 7-AVCA and adding acid.

Abstract translation: 目的：提供具有新晶体的7-氨基-3-乙烯基头孢菌素酸盐水合物及其制备方法，以工业合成高产率和高纯度的新型结晶7-AVCA水合物。 构成：具有新颖结晶的化学式1的7-氨基-3-乙烯基头孢菌素酸盐水合物在8.98±0.3,18.06±0.3,28.95±0.3,32.32±0.3,33.76±0.3和34.40±0.3的特征峰 。 制备结晶7-氨基-3-乙烯基头孢菌素酸盐水合物的方法包括：向对甲氧基苄基-7-苯基乙酰氨基-3-乙烯基-3-头孢呋喃-4-羧酸甲酯中加入甲酚或苯酚并搅拌以脱保护 羧基保护基; 用碱调节pH值，加入cinta CELC-PA酶去保护氨基保护基; 通过用无机酸调节pH使得脱保护的7-AVCA结晶的步骤; 并向7-AVCA中加入甲醇溶液和碱并加入酸的步骤。

公开(公告)号：KR1020090073659A

公开(公告)日：2009-07-03

申请号：KR1020070141668

申请日：2007-12-31

Applicant: 한국과학기술연구원

Inventor： 오창현 ,  조정혁 ,  조남현 ,  안광일 ,  천기정 ,  이교철 ,  문병석 ,  최태현 ,  구대호

IPC: C07D405/04 ,  C07H15/22

Abstract: A manufacturing method for manufacturing a 2-deoxy-2-[18F]fluoro-5-methyl-1-beta-L-arabinofuranosyluracil compound is provided to produce a compound having high intake rate by specifically activating in a cell line which HSV-TK gene is specifically expressed. A 2-deoxy-2-[18F]fluoro-5-methyl-1-beta-L-arabinofuranosyluracil compound is denoted by the chemical formula 1. A method for manufacturing the 2-deoxy-2-[18F]fluoro-5-methyl-1-beta-L-arabinofuranosyluracil compound comprises: a step of reacting anhydrous trifluoro methanesulfonyl in a compound of the chemical formula 2 under the presence of organic solvent to produce the tribenzoyl triflate saccharide compound of the chemical formula 3; a step of introducing fluorine-18 to produce a compound of the chemical formula 4; a step of reacting the compound of the chemical formula 4 with anhydrous acetic acid under the presence of organic solvent to produce a compound of the chemical formula 5; a step of reacting the compound of the chemical formula 5 with silylated thymine to produce a compound of the chemical formula 7; and a step of hydrolyzing the compound of the chemical formula 7 to produce the compound of the chemical formula 1.

Abstract translation: 提供了制备2-脱氧-2- [18 F]氟-5-甲基-1-β-L-阿拉伯呋喃糖尿嘧啶化合物的制备方法，通过在细胞系中特异性活化以产生高摄入率的化合物，其中HSV-TK 基因被特异表达。 2-脱氧-2- [18 F]氟-5-甲基-1-β-L-阿拉伯呋喃糖尿嘧啶化合物由化学式1表示。制备2-脱氧-2- [18 F]氟-5- 甲基-1-β-L-阿拉伯呋喃糖尿嘧啶化合物包括：在有机溶剂的存在下，使化学式2的化合物中的无水三氟甲烷磺酰化反应生成化学式3的三苯甲酰基三氟甲磺酸酯化合物的步骤; 引入氟-18以制备化学式4的化合物的步骤; 在有机溶剂的存在下使化学式4的化合物与无水乙酸反应以产生化学式5的化合物的步骤; 使化学式5的化合物与甲硅烷基化的胸腺嘧啶反应以产生化学式7的化合物的步骤; 以及水解化学式7的化合物以制备化学式1的化合物的步骤。