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    세팔로스포린 유도체의 제조방법
    2.
    发明授权
    세팔로스포린 유도체의 제조방법 失效
    制备CEPHOROSPORIN衍生物的方法

    公开(公告)号：KR1019890000523B1

    公开(公告)日：1989-03-20

    申请号：KR1019860003550

    申请日：1986-05-07

    Applicant: 한국과학기술연구원

    Inventor： 김완주 ,  장문호 ,  김봉진 ,  김성각

    IPC: C07D501/24 ,  C07D501/26

    CPC classification number: C07D501/36 ,  C07D501/32

    Abstract: Cephalosporins (I)[R1=H, CHO; X=(II) or O2CCH3 were prepd.. Thus, 7- amino-3-(1-methyl-1H-tetrazol-5-ylthiomethyl)-3-cephem-4carboxylic acid and monotrimethylacetamide in ethylacetate was heated for 50min at 50≦̸C, cooled to >=-15≦̸C, and then reacted with a mixt. of D- mandelic acid formate ester and diphenyl-2-pyridone1-phosphate in triethylamine for 150min at 50≦̸C with stirring. The reaction mixt. was extd. with ethylacetate/H2O (1:1) and filtered. The aq. phase extd. with ethylacetate and org. phase pooled, washed with 5% HNO3 and satd. NaCl over 2 times, resptly.. The org. phase was dried on MgSO4, filtered, vacuum-evapd, and crystallized with ethylacetate/n- hexane.

    Abstract translation: 头孢菌素（I）[R1 = H，CHO; 因此，将7-氨基-3-（1-甲基-1H-四唑-5-基硫甲基）-3-头孢烯-4-羧酸和单三乙基乙酰胺在乙酸乙酯中的混合物在50℃加热50分钟; C，冷却至> = -15℃，然后与混合物反应。 的D-扁桃酸甲酸酯和二苯基-2-吡啶酮-1-磷酸酯在三乙胺中在50℃和150℃搅拌150分钟。 反应混合 被释放 用乙酸乙酯/ H 2 O（1:1）洗涤并过滤。 水。。 相变 与乙酸乙酯和组织。 阶段合并，用5％HNO3和satd洗涤。 NaCl超过2次， 相用MgSO 4干燥，过滤，真空蒸发，用乙酸乙酯/正己烷结晶。

    세팔로스포린 유도체의 제조방법
    4.
    发明授权
    세팔로스포린 유도체의 제조방법 失效
    制备CEPHOROSPORIN衍生物的方法

    公开(公告)号：KR1019890002216B1

    公开(公告)日：1989-06-23

    申请号：KR1019870001884

    申请日：1987-03-03

    Applicant: 한국과학기술연구원

    Inventor： 장문호 ,  최경일 ,  김성각

    IPC: C07D501/34

    Abstract: Cephalosporin derivs. (of formula (I), R1=C1-4 aliphatic alkyl) are new. Thus, suspend 7-amino-3-carbamoyloxymethyl-3cephem-4-carboxylic acid 2.73g into ethylacetate 75mL, add N-trimethylsyllylacetamide 5.20g at 30-35 deg.C with stirring (1.5 hr), cool to 1-3 deg.C, add 2-(fur-2-yl)-2-methoxyiminoacetic acid 1.86g, diphenyl-2-pyridon-1- yl-phosphate 3.77g and (Et)3N 1.53ml sequently at same temp. and stir for 3.5hr, add ethylacetate 80ml and water 80ml, adjust pH to 2.0 with 2N HCl and stir for 1hr at 0-5 deg.C to give 3- carbamoyloxymethyl-7-2-(fur-2-yl)2-methoxyiminoacetamide-ceph-3-em-4- carboxylic acid 3.86g (87.5% yield).

    Abstract translation: 头孢菌素衍生物。 （式（I），R1 = C1-4脂族烷基）是新的。 因此，将7-氨基-3-氨基甲酰氧基甲基-3-头孢烯-4-羧酸2.73g悬浮于乙酸乙酯75mL中，在30-35℃，搅拌（1.5小时）下加入5.20g N-三甲基甲酰基乙酰胺，冷却至1-3℃。 在相同温度下，依次加入2-（呋喃-2-基）-2-甲氧基亚氨基乙酸1.86g，二苯基-2-吡啶酮-1-基 - 磷酸酯3.77g和（Et）3 N 1.53ml。 并搅拌3.5小时，加入乙酸乙酯80ml和水80ml，用2N HCl将pH调节至2.0，在0-5℃下搅拌1小时，得到3-氨基甲酰氧基甲基-7-2-（呋喃-2-基）-2- 甲氧基亚氨基乙酰胺 - 头孢-3-烯-4-羧酸3.86g（收率87.5％）。

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