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    One-pot process for preparation of 7beta-amino- and 7beta-acylamino- 3-substituted methyl-3-cephem-4-carboxylic acid derivatives and process for deoxygenation of 7beta-acylamino-3-cephem-4-carboxylic acid 1-oxide derivatives
    1.
    发明公开
    One-pot process for preparation of 7beta-amino- and 7beta-acylamino- 3-substituted methyl-3-cephem-4-carboxylic acid derivatives and process for deoxygenation of 7beta-acylamino-3-cephem-4-carboxylic acid 1-oxide derivatives 失效
    一锅法7β-氨基和脱氧7的β-酰氨基-3-取代的甲基-3-头孢烯-4-羧酸化合物和方法的制备7-β-酰氨基-3-头孢烯-4-羧酸-1- -oxyd化合物。

    公开(公告)号：EP0137534A2

    公开(公告)日：1985-04-17

    申请号：EP84201215.5

    申请日：1984-08-24

    申请人： GIST-BROCADES N.V.

    发明人： Verweij, Jan ,  Grootveld, Herman Hendrik ,  Hirs, Henri Gerard Julius ,  van Veen, Gerardus Johannes ,  Kalter, Jan ,  Henniger, Peter Wolfgang

    IPC分类号： C07D501/04 ,  C07D501/18 ,  C07D501/20

    CPC分类号： C07D501/04

    摘要： Multi-step one-pot process for the preparation of inter alia 7β-amino- and 7β-acylamino-3-substituted methyl-3-cephem-4-carboxylic acid derivatives starting from 7p-acylamino-3-methyl-3-cephem-4-carboxylic acid 1β-oxide derivatives, comprising a new process for deoxygenation of generally 7p-acylamino-3-cephem-4-carboxylic acid 1-oxide derivatives optionally substituted in the 7a-position, which can be applied as single step or can be incorporated in multistep processes without isolation of intermediates.
    The deoxygenation involves the use of phosphorus pentachloride and an olefine for removal of chlorine at least in part by addition to carbon-carbon double bond.
    Preferred aspects are lasting protection of reactive substituents by silylation and preparation on industrial scale of generally 7β-amino-3-heterocyclic thiomethyl-3-cephem-4-carboxylic acids starting from suitably 7p-phenylacetamido-3-methyl-3-cephem-4-carboxylic acid 9β-oxide.

    摘要翻译： 用于制备多步一锅法，尤其7测试 - 氨基和7的β酰氨基-3- substituiertem甲基-3-头孢烯-4-羧酸的从7测试起始酸衍生物酰氨基-3-甲基-3- -cephem -4-羧酸1的β氧化物衍生物，包括一个新的流程用于基因反弹的脱氧7测试酰氨基-3-头孢烯-4-羧酸1-氧化物衍生物在α位7或者substituiertem，其可以是 应用为单一步骤，或可以在多步工艺中掺入不分离中间体的。 ... 脱氧涉及通过除碳 - 碳双键部分的使用五氯化磷和烯烃用于去除至少氯的。 ... 优选的方面是通过甲硅烷基化并制备基因反弹工业规模持久反应性取代基保护7测试氨基-3-杂环从适当7测试苯基乙酰氨基起始硫甲基-3-头孢烯-4-羧酸 3-甲基-3-头孢烯-4-羧酸1的β氧化物。

    Process for the preparation of a (D-alpha-amino-(p-hydroxyphenyl)-acetamido) group containing cephalosporanic acid derivatives
    3.
    发明公开
    Process for the preparation of a (D-alpha-amino-(p-hydroxyphenyl)-acetamido) group containing cephalosporanic acid derivatives 失效
    Verfahren zur Herstellung von eine（D-α-氨基 - （对羟基苯基） - 乙酰氨基）-Gruppe enthaltendenCephalosporansäure-Derivaten。

    公开(公告)号：EP0019345A1

    公开(公告)日：1980-11-26

    申请号：EP80200702.1

    申请日：1978-08-11

    申请人： GIST-BROCADES N.V.

    发明人： Henniger, Peter Wolfgang ,  Van Der Drift, Johannes Karel ,  Van Veen, Gerard Joannes ,  Kapur, Jagdish Chander

    IPC分类号： C07D501/06

    CPC分类号： C07D499/00

    摘要： Process for the preparation of [D-a-amino-(p- hydroxyphenyl)acetamido] groups containing cephalosporanic acid derivatives, comprising the acylation of a compound of the formulae:
    wherein R,, R 2 and R 3 representthe same or a different group and may be selected from a lower alkyl, benzyl, cycloalkyl or. phenyl-group and preferably lower alkyl and more preferably a methyl group an wherein X represents a residue selected from the group consisting of hydrogen, acetoxy or a five-membered heterocyclic thio residue, containing heteroatoms selected from nitrogen, oxygen, and/or sulphur and optionally substituted by lower alkyl and wherein an eventually present -NH- radical has optionally been silylated, which compound is previously prepared by the reaction of 7-aminocephalosporanic acid or its 3-methyl modifications with at least one equivalent and preferably about two with respect to other 3-methyl modifications of 7-ACA of a tri(lower)alkyl silyl groups supplying agent in a dry, inert, water insoluble solvent, such as methylene chloride, by rapid mixing of a pre-cooled solution of the compound offormulae I and Il with a pre-cooled reaction mixture of at least an equimolecular amount of a compound of the formula


    wherein R 4 represents lower alkyl and preferably methyl,
    R 5 represents hydrogen or lower alkyl and preferably methyl,
    R 6 represents lower alkoxy and preferably methoxy,

    and R 7 represents lower alkoxy and preferably methoxy, previously prepared from the corresponding Dane salt and an acid chloride under anhydrous conditions in the presence of a tertiary amine as catalyst, such as N-methylmorpholine in a dry, inert, water insoluble, organic solvent such as methylene chloride mixed with a co-solvent or methyl isobutylketone or tetrahydrofuran optionally mixed with a co-solvent, and the continuation of the reaction at a temperature of -10°C or lower and preferably from -20°C to -30°C whereafter the desired compound is recovered by usual methods.

    摘要翻译： 制备含有头孢菌酸衍生物的[D-α-氨基 - （p-羟基苯基）乙酰氨基]基团的方法，包括下式化合物的酰化：其中R 1，R 2和R 3表示相同或不同的 并且可以选自低级烷基，苄基，环烷基或苯基，优选选自低级烷基，更优选甲基，其中X表示选自氢，乙酰氧基或五元杂环硫基残基的残基 ，其含有选自氮，氧和/或硫并且任选被低级烷基取代的杂原子，并且其中最终存在的-NH-基团任选被甲硅烷基化，该化合物预先通过7-氨基头孢烷酸或其3- 相对于三（低级）烷基甲硅烷基供给剂的7-ACA的其它3-甲基修饰物，在干燥， 惰性的水不溶性溶剂如二氯甲烷，通过将式I和II化合物的预冷却的溶液与至少等摩尔量的式CHEM的化合物的预冷反应混合物快速混合， 其中R4表示低级烷基，优选甲基，R5表示氢或低级烷基，优选甲基，R6表示低级烷氧基，优选甲氧基，R7表示低级烷氧基，优选甲氧基，预先由相应的丹烷盐和酰氯在无水条件下制备 在作为催化剂的叔胺如N-甲基吗啉存在下，在干燥，惰性，不溶于水的有机溶剂如二氯甲烷中混合，与共溶剂或甲基异丁基酮或四氢呋喃混合，任选与共溶剂混合，以及 在-10℃或更低的温度下，优选在-20℃至-30℃下继续反应，然后通过常规方法回收所需化合物 方法。

    Process for the preparation of 6- D-alpha-amino-(p-hydroxyphenyl)-acetamido penicillanic acid
    4.
    发明公开
    Process for the preparation of 6- D-alpha-amino-(p-hydroxyphenyl)-acetamido penicillanic acid 失效
    Verfahren zur Herstellung von 6-D-α-氨基 - （对羟基苯基） - 乙酰氨基青霉素。

    公开(公告)号：EP0001133A1

    公开(公告)日：1979-03-21

    申请号：EP78200140.8

    申请日：1978-08-11

    申请人： GIST-BROCADES N.V.

    发明人： Henniger, Peter Wolfgang ,  Van Der Drift, Johannes Karel ,  Van Veen, Gerard Joannes

    IPC分类号： C07D499/12 ,  C07D499/68

    CPC分类号： C07D499/00

    摘要： Process for the preparation of / D-a-amino-p- hydrox- yphenylacetamido/ groups containing penicillanic acid and cephalosporanic acid derivatives, comprising the acylation of a compounds of the formulae:
    and/or
    or
    and/or
    wherein R 1 , R 2 , and R 3 represent the same or a different group and may be selected from a lower alkyl, benzyl, cycloalkyl or phenyl-group and preferably lower alkyl and more preferably a methyl group and wherein X represents a residue selected from the group consisting of hydrogen, acetoxy or a fivemembered heterocyclic thio residue, containing heteroatoms selected from nitrogen, oxygen and/or sulphur and optionally substituted by lower alkyl and wherein an eventually present -NH- radical has optionally been silylated, which compound is previously prepared by the reaction of -6-aminopenicillanic acid or 7-aminocephalosporanic acid or its 3-methyl modifications with at least one equivalent and preferably about 2 with respect to 6-APA, 7-ACA or 7-ADCA and about 3 equivalents with respect to other 3-methyl modifications of 7-ACA of a tri(lower)alkyl silyl groups supplying agent in a dry inert, water insoluble solvent, such as methylene chloride, by rapid mixing of a pre-cooled solution of the compound of formula I-IV with a pre-cooled reaction mixture of at least an equimolar amount of a compound of the formula
    wherein R 4 represents lower alkyl and preferably methyl, R 5 represents hydrogen or lower alkyl and preferably methyl, R 6 represents lower alkoxy and preferably methoxy and R 7 represents lower alkoxy and preferably methoxy, previously prepared from the corresponding Dane salt and an acid chloride under anhydrous conditions in the presence of a tertiary amine as catalyst, such as N-methylmorpholine in a dry, inert, water insoluble, organo solvent such as methylene chloride mixed with a cosolvent or methyl isobutylketone or tetrahydrofuran optionally mixed with a cosolvent, and the continuation of the reactior at a temperature of -10°C or lower and preferably from 2°C to 30°C whereafter the desired compound is recovered by usual methods.

    摘要翻译： 制备/ D-氨基 - 对 - 羟基苯基乙酰氨基/含有青霉烷酸和头孢菌酸衍生物的基团的方法，包括下式化合物的酰化：其中R 1，R 2和R 3表示相同或不同的 并且可以选自低级烷基，苄基，环烷基或苯基，优选选自低级烷基，更优选甲基，其中X表示选自氢，乙酰氧基或五元杂环硫代残基的残基，其含有 选自氮，氧和/或硫并且任选被低级烷基取代的杂原子，并且其中最终存在的-NH-基团任选被甲硅烷基化，该化合物预先通过6-氨基青霉烷酸或7-氨基头孢烷酸或其 相对于6-APA，7-ACA或7-ADCA具有至少一个当量，优选约2个的3-甲基修饰和约3当量， 对于三（低级）烷基甲硅烷基供体试剂在干惰性，不溶于水的溶剂如二氯甲烷中的7-ACA的其它3-甲基修饰，通过快速混合式 I-IV与至少等摩尔量的式CHEM化合物的预冷反应混合物，其中R 4表示低级烷基，优选甲基，R 5表示氢或低级烷基，优选甲基，R 6表示低级烷氧基，优选 甲氧基，R7表示低级烷氧基，优选甲氧基，预先由相应的丹烷盐和酰氯在无水条件下，在作为催化剂的叔胺如N-甲基吗啉存在下，在干燥，惰性，不溶于水的有机溶剂 例如与助溶剂混合的二氯甲烷或与共溶剂任选混合的甲基异丁基酮或四氢呋喃，并在-10℃或更低的温度下继续反应 优选为20℃〜30℃，通过常规方法回收所需化合物。