[EN] INTERMEDIATES FOR THE SYNTHESIS OF 1,2-BIS(4,7-DIMETHYL-1,4,7-TRIAZACYCLONON-1-YL)-ETHANE AND PREPARATION METHOD THEREOF<br/>[FR] INTERMÉDIAIRES POUR LA SYNTHÈSE DE 1,2-DI(4,7-DIMÉTHYL-1,4,7-TRIAZACYCLONON-1-YL)-ÉTHANE, ET PROCÉDÉ D'ÉLABORATION CORRESPONDANT
申请人:UNILEVER PLC
公开号:WO2012003598A1
公开(公告)日:2012-01-12
The present invention provides intermediates for the synthesis of 1,2-bis(4,7-dimethyl-1,4,7-triazacyclonon-1-yl)-ethane and preparation method thereof. The intermediates are protonated salts of 1,4-ditosylate-1,4,7-triazacyclononane or 1,4-dibenzenesulphonate-1,4,7-triazacyclononane. The preparation method of 1,4-diarylsulfonate-1,4,7-triazacyclononane (compound A) comprises reacting 1,4,7-triarylsulfonate-1,4,7-triazacyclononane (compound B) in an acidic medium comprising sulphuric acid, wherein the molar ratio of B to sulphuric acid is in the range from 1 : 0.5 to 1 : 10, or reacting 1,4,7-triarylsulfonate-1,4,7-triazacyclononane (compound B) in an acidic medium and working up the acidic medium when the conversion of B to A is at least 50 mol % yielding compound A.
本发明提供了合成1,2-双(4,7-二甲基-1,4,7-三氮杂环辛-1-基)-乙烷的中间体及其制备方法。这些中间体是1,4-二对甲苯磺酸盐-1,4,7-三氮杂环辛烷或1,4-二苯基磺酸盐-1,4,7-三氮杂环辛烷的质子化盐。1,4-二芳基磺酸盐-1,4,7-三氮杂环辛烷(化合物A)的制备方法包括在含硫酸的酸性介质中反应1,4,7-三芳基磺酸盐-1,4,7-三氮杂环辛烷(化合物B),其中B与硫酸的摩尔比在1:0.5到1:10的范围内,或在酸性介质中反应1,4,7-三芳基磺酸盐-1,4,7-三氮杂环辛烷(化合物B),当B转化为A的转化率至少为50摩尔%时,处理酸性介质,得到化合物A。