摘要
分别采用硝酸-硝酸钾、发烟硫酸-硝酸钾、发烟硫酸-硝酸钠和发烟硫酸-硝酸铵4种超酸体系对六乙酰基六氮杂异伍 烷(HAIW)进行硝化,合成了六硝基六氮杂异伍 烷(HNIW),属首次用超酸硝化方法合成HNIW。通过实验得到最佳硝化反应条件,以发烟硫酸-硝酸钾超酸体系为硝化剂,当温度为70℃,反应时间为3 5h,目标产物的最高得率为83 1%,质量分数达到98%以上(达到应用的纯度)。同时对超酸硝化N双取代的酰胺类化合物HAIW的反应机理进行了探讨,超酸体系中含有高浓度的硝酰正离子(NO2+),在该反应中NO2+是进攻酰胺氮原子的有效基团。
Hexanitrohexaazaisowurtzitane (HNIW) or 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetrocyclo-[5.5.0.0^(5,9).0^(3,11)] dodecane was synthesized at 70 ℃ in 3.5 hour from hexaacetylhexaazaisowurtzitane (HAIW) with super acids (i.e.nitric acid/potassium nitrate,oleum/potassium nitrate,oleum/sodium nitrate and oleum/ammonium nitrate) for the first time.The highest yield was 83.1% and the purity was over 98%.The possible mechanism of the reaction between HAIW and super acids (being oleum/nitrate) was discussed.The NO^+_2 in the super acid at high concentration is regarded as the effective group to attack the nitrogen atoms of HAIW molecule.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2004年第5期321-323,共3页
Fine Chemicals
基金
国防科工委预研基金资助项目(12060451867)
