| 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 |
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| 引用本文： | 魏俊发,石先莹,何地平,张勇. 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[J]. 有机化学, 2003, 23(10): 1142-1145 |
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| 作者姓名： | 魏俊发 石先莹 何地平 张勇 |
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| 作者单位： | 魏俊发（陕西师范大学化学与材料科学学院,西安,710062） 石先莹（陕西师范大学化学与材料科学学院,西安,710062） 何地平（陕西师范大学化学与材料科学学院,西安,710062） 张勇（陕西师范大学化学与材料科学学院,西安,710062） |
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| 基金项目： | 国家自然科学基金(No.20172036)和教育部骨干教师基金[No.教技司(2000)65号]资助项目. |
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| 摘 要： | 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。
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| 关 键 词： | 氮杂环化合物 对甲苯碘酰胺 水解 酰化 |
| 修稿时间： | 2002-12-06 |
A Rapid Detosylation of N,N',N",N"'-Tetra(p-tosyl)-1,4,7,10- tetraazacyclododecane under Microwave Irradiation and Normal Pressure |
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| Affiliation: | School of Chemistry and Material Science, Shaanxi Normal University |
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| Abstract: | 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. |
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| Keywords: | NITROGEN HETEROCYCLICS p-tolunosulfamide HYDROLYSIS ACYLATION |
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