六氮杂异伍兹烷衍生物的选择性硝解

化工进展

六氮杂异伍兹烷衍生物的选择性硝解

宋海香，王艳飞，张艳维，赵亮

安阳工学院化学与环境工程系

出版日期:2009-09-05 发布日期:2009-09-05

Selective nitration of a hexazaisowurzitane derivative

SONG Haixiang，WANG Yanfei，ZHANG Yanwei，ZHAO Liang

Department of Chemical and Environmental Engineering，Anyang Institute of Technology

Online:2009-09-05 Published:2009-09-05

摘要/Abstract

摘要： 以六氮杂异伍兹烷衍生物：四乙酰基-二(对氯苯甲酰基)六氮杂异伍兹烷（TABIW）为基质，经选择性硝解合成了四硝基-二(3,5-二硝基-4-氯苯甲酰基)六氮杂异伍兹烷（TANIW），分别用FTIR、1H NMR及元素分析对产物TANIW进行了结构表征，并讨论了硝解剂、硝解温度、硝解时间、加料方式对反应的影响。结果表明：冰浴下，在搅拌作用下分批把反应物TABIW加入到发烟硝酸[m(HNO3)=98%]中，使之溶解。待溶解完全后，慢慢滴加发烟硫酸[m(SO3)=20%]，待滴加完毕后首先升温至70 ℃并恒温反应1h，然后再升温至90 ℃并恒温反应3 h使反应完全，直接过滤得到产物，熔点为242～244 ℃，收率为71.4%。

Abstract: Selective nitration of a hexazaisowurzitane derivative，tetraacety-bis(p-chlorobenzamido) hexaazaisowurtzitane (TABIW)，was studied. Structure of the product has been determined by FTIR， 1H NMR and elemental analysis. The effect of nitration agent，reaction temperature，reaction time，feeding mode on the product yield and purity were investigated. The optimized conditions were found as：in an ice bath，the substrate was added in batches into fuming nitric acid [m(HNO3)=98%] under stirring. When the substrate was completely solubilized，oleum [m(SO3)=20%] was dropwise added. The reaction was conducted at 70 ℃ for 1h，then at 90 ℃for 3 h. Upon filtration，the target product was obtained with a yield of 71.4%，the melting point of the product was measured as 242—244℃.

宋海香，王艳飞，张艳维，赵亮. 六氮杂异伍兹烷衍生物的选择性硝解 [J]. 化工进展.

SONG Haixiang，WANG Yanfei，ZHANG Yanwei，ZHAO Liang. Selective nitration of a hexazaisowurzitane derivative[J]. Chemical Industry and Engineering Progree.