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    • 8. 发明申请
    • SYNTHESIS OF 1,4,7-TRIAZACYCLONONANE DERIVATIVES
    • 1,4,7-三氮杂萘衍生物的合成
    • WO1994000439A1
    • 1994-01-06
    • PCT/EP1993001550
    • 1993-06-16
    • UNILEVER PLCUNILEVER NV
    • UNILEVER PLCUNILEVER NVMADISON, Stephen, AlanBATAL, David, John
    • C07D255/02
    • C07D255/02Y02P20/55
    • 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.
    • 描述了用于获得三氮杂环壬烷(I),特别是1,4,7-三甲基-1,4,7-三氮杂环壬烷的改进方法。 第一步涉及在具有无机碱的水性介质中使二亚乙基三胺(DET)与磺酰化剂反应形成磺酰胺化的DET。 在第二步中,但优选在不分离中间体的相同反应器容器内,在环化单元例如乙二醇二甲苯磺酸酯或二溴乙烷存在下,将磺酰胺化的DET含水混合物与非质子有机溶剂接触,由此导致环化磺酰胺化 三胺化合物。 此后,除去保护基团,并将胺烷基化,优选在单个反应容器内,而不分离中间体。