Synthesis of a tetraamido macrocycle ligand
    14.
    发明授权
    Synthesis of a tetraamido macrocycle ligand 失效
    四氨基大环配体的合成

    公开(公告)号:US6127536A

    公开(公告)日:2000-10-03

    申请号:US318410

    申请日:1999-05-25

    IPC分类号: C07D257/10 C07D225/00

    CPC分类号: C07D257/10

    摘要: An improved synthesis for preparing a tetraamido-macrocyclic ligand, such as 5,6-Benzo-3,8,11,13-tetraoxo-2,2,9,9-tetramethyl-12,12-diethyl-1,4,7,10-tetraazacyclotridecane, H.sub.4, in greatly improved yield and in a commercially viable manner, comprising the steps of dissolving a quantity of a 1,2-bis(2-aminoalkanamido)benzene in a solution comprised of ethyl acetate and methylene chloride to yield a first reaction solution; dissolving a quantity of a malonyl dihalide in an ethyl acetate solution to yield a second reaction solution; adding the first reaction solution and the second reaction solution to a reaction vessel containing a third reaction solution comprised of refluxing ethyl acetate solution and an acid scavenger to form a reaction mixture; and isolating a solid product comprised of the tetraamido-macrocycle directly from the reaction mixture by filtration.

    摘要翻译: 用于制备四氨基 - 大环配体的改进的合成物,例如5,6-苯并-3,8,11,13-四氧代-2,2,9,9-四甲基-1,12,12-二乙基-1,4,7 ,10-四氮杂环十二烷,H4,以大大提高的产率和商业上可行的方式,包括以下步骤:将一定数量的1,2-双(2-氨基烷酰胺)苯溶解在由乙酸乙酯和二氯甲烷组成的溶液中以产生 第一反应溶液; 将一定数量的丙二酰二卤化物溶于乙酸乙酯溶液中以产生第二反应溶液; 将第一反应溶液和第二反应溶液加入到含有回流乙酸乙酯溶液和酸清除剂的第三反应溶液的反应容器中以形成反应混合物; 并通过过滤直接从反应混合物中分离由四氨基 - 大环化合物组成的固体产物。

    Synthesis of a tetraamido macrocycle ligand from a novel diamidodiol
    16.
    发明授权
    Synthesis of a tetraamido macrocycle ligand from a novel diamidodiol 失效
    从新型二酰氨基二醇合成四氨基大环配体

    公开(公告)号:US06384279B1

    公开(公告)日:2002-05-07

    申请号:US09943536

    申请日:2001-08-30

    IPC分类号: C07C23102

    CPC分类号: C07C233/18 C07D257/02

    摘要: A new composition of matter for a diamidodiol and a method for preparing the diamidodiol. The exemplary diamidodiol has the formula C15H30N2O4 and is prepared by reacting a first quantity of 2-amino-2-methyl-1-propanol with a second quantity of a di-substituted malonyl dichloride (i.e., diethylmalonyl dichloride), preferably in ethyl acetate as solvent. A tetraamido macrocycle is prepared from the diamidodiol in two steps by oxidizing the diamidodiol to form a diacid followed by coupling using a known procedure of the diacid with an aryl diamine (e.g., 1,2-diaminobenzene) to yield the tetraamido macrocycle.

    摘要翻译: 二酰氨基二醇的新物质组合物和二酰胺二醇的制备方法。 示例性二酰氨基二醇具有式C 15 H 30 N 2 O 4,并且通过使第一量的2-氨基-2-甲基-1-丙醇与第二量的二取代丙二酰氯(即二乙基丙二酰氯)反应,优选在乙酸乙酯中反应制备,如 溶剂。 通过氧化二酰氨基二醇以形成二酸,然后使用二酸的已知方法与芳基二胺(例如1,2-二氨基苯)偶合,从二酰氨基二醇制备四酰氨基大环化合物,得到四酰胺大环化合物。

    Synthesis of a tetraamido macrocycle ligand from a novel diamidodiol
    17.
    发明授权
    Synthesis of a tetraamido macrocycle ligand from a novel diamidodiol 有权
    从新型二酰氨基二醇合成四氨基大环配体

    公开(公告)号:US06297400B1

    公开(公告)日:2001-10-02

    申请号:US09347435

    申请日:1999-07-02

    IPC分类号: C07C23303

    CPC分类号: C07C233/18 C07D257/02

    摘要: A new composition of matter for a diamidodiol and a method for preparing the diamidodiol. The exemplary diamidodiol has the formula C15H30N2O4 and is prepared by reacting a first quantity of 2-amino-2-methyl-1-propanol with a second quantity of a di-substituted malonyl dichloride (i.e., diethylmalonyl dichloride), preferably in ethyl acetate as solvent. A tetraamido macrocycle is prepared from the diamidodiol in two steps by oxidizing the diamidodiol to form a diacid followed by coupling using a known procedure of the diacid with an aryl diamine (e.g., 1,2-diaminobenzene)to yield the tetraamido macrocycle.

    摘要翻译: 二酰氨基二醇的新物质组合物和二酰胺二醇的制备方法。 示例性二酰氨基二醇具有式C 15 H 30 N 2 O 4,并且通过使第一量的2-氨基-2-甲基-1-丙醇与第二量的二取代丙二酰氯(即二乙基丙二酰氯)反应,优选在乙酸乙酯中反应制备,如 溶剂。 通过氧化二酰氨基二醇以形成二酸,然后使用二酸的已知方法与芳基二胺(例如1,2-二氨基苯)偶合,从二酰氨基二醇制备四酰氨基大环化合物,得到四酰胺大环化合物。