1,4,7,10—四氮杂环十二烷的制备

IMPROVED PREPARATION OF 1, 4, 7, 10—TETRAAZACYCLO DODECANE

N,N′,N″—三(对—甲苯磺酰基)二亚乙基三胺与氢化钠反应生成二钠盐,然后与N,O,O'—三(对—甲苯磺酰基)双(2—羟乙基)胺进行缩合环化反应,得N—对甲苯磺酰化的四氮杂环十二烷。在浓H_2SO_4作用下,脱去对—甲苯磺酰基,最后得到了1,4,7,10—四氮杂环十二烷,总得率为44％。

N, N', N'—Tris(p—toluenesulfonyl)-diethylenetfiamine reacted with sodium hydride to produce its disodium salt, which was convered to 1, 4, 7, 10—tetrakis (p—tolysufonyl)—1, 4, 7, 10—tetraazacyclododecane by condensation—cyclization with N, O, O'-tfis (p-toluenesulfonyl)bis (2-hydroxylethyl)amine. 1, 4, 7, 10—Tetraazacyclododecane was prepared by the detosylation of the tosylated cyclic amine in the presence of sulfuric acid. The total yieid was 44％。