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有机化学
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有机化学 ›› 2003, Vol. 23 ›› Issue (10): 1142-1145. 上一篇    下一篇

研究论文

N,N',N",N"'-四对甲苯碘酰-1，4，7，10-四氮杂环十二烷的微小常压快速水解

魏俊发;石先莹;何地平;张勇   

  1. 陕西师范大学化学与材料科学学院
  • 发布日期:2003-10-25

A Rapid Detosylation of N,N',N",N"'-Tetra(p-tosyl)-1,4,7,10- tetraazacyclododecane under Microwave Irradiation and Normal Pressure

Wei Junfa;Shi Xianying;He Diping;Zhang Yong   

  1. School of Chemistry and Material Science, Shaanxi Normal University
  • Published:2003-10-25

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N,N',N",N"'-四对甲苯磺酰-1，4，7，10-四氮杂环十二烷是Atkins法合成1， 4，7，10-四氮杂环十二烷的关键中间体，但其水解脱磺酰基比较困难，常规水解 一般需要采用96%-98%硫酸在140 ℃左右加热2-3d。报道了一种微波促进快速水解 法，即在稍加改装或未改装的家用微波炉中，采用95%-98%硫酸，控制火力2-5档， 全对甲苯碘酰化全氮冠醚仅需50-120 s即可完成水解，比常规加热水解所需时间缩 短约3000-8000倍，浓硫酸用量也比常规加热水解少，收率较常规水解高。

关键词: 氮杂环化合物, 对甲苯碘酰胺, 水解, 酰化

An efficient and rapid detosylation of N,N',N", A'""-tetra(p-tosyl)- 1,4,7,10-tetraazacyclododecane, the key intermediates in Atikins' route for preparing 1,4,7,10-tetraazacyclododecane, has been investigated by hydrolysis in concentrated sulfuric acid under microwave irradiation condition in a simply refitted domestic microwave oven equipped with an electromagnetic stirrer and a refluxing condenser. The results indicated that the hydrolysis and detosylation of poly(p-tosyl) compounds were completed within 50～120 s in 95%～98% sulfuric acid under the irradiation power of 75～375 W. In comparison with the common hydrolysis which was completed for 2～3 d at 14℃ in 96%～98% sulfuric acid, the microwave irradiation accelerated (MIA) hydrolysis is rather rapid.

Key words: NITROGEN HETEROCYCLICS, p-tolunosulfamide, HYDROLYSIS, ACYLATION

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