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    SYNTHESIS OF 1,4,7-TRIAZACYCLONONANE DERIVATIVES
    8.
    发明公开
    SYNTHESIS OF 1,4,7-TRIAZACYCLONONANE DERIVATIVES 失效
    1,4,7-三氮杂环壬烷衍生物的合成

    公开(公告)号：EP0648211A1

    公开(公告)日：1995-04-19

    申请号：EP93914669.0

    申请日：1993-06-16

    申请人： UNILEVER PLC ,  UNILEVER N.V.

    发明人： MADISON, Stephen, Alan ,  BATAL, David, John

    IPC分类号： C07D255

    CPC分类号： C07D255/02 ,  Y02P20/55

    摘要： An improved process is described for obtaining triazacyclononanes (I), especially 1,4,7-trimethyl-1,4,7-triazacyclononane. The first step involves reacting diethylenetriamine (DET) with a sulfonylation agent to form a sulfonamidated DET, in an aqueous medium with an inorganic base. In a second step, but preferably within the same reactor vessel without isolating intermediates, the sulfonamidated DET aqueous mixture is contacted with an aprotic organic solvent in the presence of a cyclizing unit such as ethylene glycol ditosylate or ethylene dibromide, thereby resulting in a cyclized sulfonamidated triamine compound. Thereafter the protecting groups are removed and the amine is alkylated, preferably within a single reaction vessel without isolation of intermediates.

    摘要翻译： 描述了获得三氮杂环壬烷（I），特别是1,4,7-三甲基-1,4,7-三氮杂环壬烷的改进方法。 第一步涉及使二亚乙基三胺（DET）与磺酰化剂反应以在具有无机碱的含水介质中形成磺酰胺化的DET。 在第二步中，但优选在没有分离中间体的同一反应容器内，使磺酰胺化的DET含水混合物在环化单元如乙二醇二甲苯磺酸酯或乙烯二溴化物存在下与非质子有机溶剂接触，由此产生环化磺酰胺化 三胺化合物。 此后，除去保护基并将胺烷基化，优选在单一反应容器内不分离中间体。