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    • 5. 发明公开
    • (1R, 5R, 6S)-p-나이트로벤질-2-(다이페닐포스포릴옥시)-6-[(R)-1-하이드록시에틸]-1-메틸-카바페넴-3-카복실레이트(MAP)결정형 Ⅱ의 제조방법
    • 制备(1R,5R,6S)-P-硝基苯基-2-二苯基膦基锂的晶体形式II的方法-6 - [(R)-1-羟基乙基] -1-甲基 - 碳酰基-3-羧酸酯
    • KR1020100052868A
    • 2010-05-20
    • KR1020080111741
    • 2008-11-11
    • 주식회사 대웅제약대웅바이오 주식회사
    • 문성철이경호송충현전선아박성우이병구최수진송윤석강필구
    • C07D487/04C07D477/20C07D413/14
    • PURPOSE: A method for preparing (1R, 5R, 6S)-p-nitrobenzyl-2-(diphenylphosphoryloxy)-6-[(R)-1-hydroxyethyl]-1-methyl-carbapenem-3-carboylate(MAP) crystalline II is provided to obtain MAP crystalline II of high purity and high yield without separate cooling process. CONSTITUTION: A method for preparing (1R, 5R, 6S)-p-nitrobenzyl-2-(diphenylphosphoryloxy)-6-[(R)-1-hydroxyethyl]-1-methyl-carbapenem-3-carboylate(MAP) crystalline II comprises: a step of dissolving (1R, 5R, 6S)-p-nitrobenzyl-2-(diphenylphosphoryloxy)-6-[(R)-1-hydroxyethyl]-1-methyl-carbapenem-3-carboylate(MAP) crystalline I in dichloromethane, chloroform, or acetone; and a step of crystallizing by dropping diethyl ether, isopropyl ether, normal hexane, normal heptanes, or cyclo hexane. The dichloromethane or chloroform is used in a volume of 2-10 times to MAP weight. The acetone is used in a volume of 2-10 times to MAP weight. The MAP crystalline I is dissolved in dichloromethane or chloroform at 5-60°C or in acetone at 30-60°C.
    • 目的:制备(1R,5R,6S)对硝基苄基-2-(二苯基磷酰氧基)-6 - [(R)-1-羟乙基] -1-甲基 - 碳青霉烯-3-甲酸酯(MAP)结晶II 被提供以获得高纯度和高产率的MAP结晶II,而不需要单独的冷却过程。 构成:制备(1R,5R,6S)对硝基苄基-2-(二苯基磷酰氧基)-6 - [(R)-1-羟乙基] -1-甲基 - 碳青霉烯-3-甲酰胺(MAP)结晶II 包括:将(1R,5R,6S)对硝基苄基-2-(二苯基磷酰氧基)-6 - [(R)-1-羟乙基] -1-甲基 - 碳青霉烯-3-甲酰胺(MAP)结晶I 在二氯甲烷,氯仿或丙酮中; 和通过滴加二乙醚,异丙醚,正己烷,正庚烷或环己烷的结晶步骤。 二氯甲烷或氯仿的使用体积为MAP重量的2-10倍。 丙酮的使用量是MAP重量的2-10倍。 MAP结晶I在30-60℃溶于二氯甲烷或氯仿或5-60℃丙酮。