桥连双-(三氮杂环壬烷)化合物的合成

Syntheses of Bis (1,4,7-triazacyclononanylmethyl) Benzene or Pyridine Ligands

利用无水碳酸钾作缩合剂,在精制乙腈中使N,N’-二对甲苯磺酰基-1,4,7-三氮杂环壬烷3与双溴甲基化合物4a～4c缩合得到N-对甲苯磺酰基取代的桥连双-(三氮杂环壬烷)5a～5c,经浓硫酸脱去氮原子上的保护基因得到桥连双-(三氮杂环壬烷)6a～6c。化合物5a～5c和6a～6c均经元素分析、IR、~1H NMR、^(13)C NMR、MS等测试手段证实其结构和组成。

The reaction of 1,4 - bis(p - toluenesulfonyl) - 1,4,7- triazacyclononane with the bis (bromomethyl) compounds 4a ~ 4c in CHsCN/KaCOs afforded the N - p - toluenesulfonyl substituted bis (1,4,7 - triazacyclononanylmethyl) compounds 5a - 5c. Treatment of compounds 5a ~ 5c with cone. H2SO4 followed by cone. HCl gave the hydrochloride of 6a ~ 6c. Compounds 5a ~ 5c and 6a ~ 6c were identified by elemental analysis and spectral analysis (IR,1H NMR,13C NMR,MS).