以四乙酰基二苄基六氮杂异伍兹烷为基质,经亚硝解脱苄合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW);用纯硝酸氧化TADNSIW制备四乙酰基二硝基六氮杂异伍兹烷(TADNIW),收率93.0%,以上两步反应均在室温下完成。在85℃条件下,TADNIW经硝...以四乙酰基二苄基六氮杂异伍兹烷为基质,经亚硝解脱苄合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW);用纯硝酸氧化TADNSIW制备四乙酰基二硝基六氮杂异伍兹烷(TADNIW),收率93.0%,以上两步反应均在室温下完成。在85℃条件下,TADNIW经硝硫混酸硝解合成了六硝基六氮杂异伍兹烷(HNIW),反应时间50 m in,收率95.1%,质量分数98.80%。用硝硫混酸对TADNSIW进行硝解合成了HNIW,并优化了反应条件,反应温度90℃,反应时间60 m in,硝解剂必须大于14 mL(底物TADNSIW 1.2 g),收率为96.1%,质量分数98.87%。分别用FTIR,1HNMR和元素分析对目标化合物进行了表征。前体TADNSIW和TADNIW分子中只有乙酰基和亚硝基,它们的硝解反应体系较简单,反应时间短、反应条件温和,母液中只含有乙酸和硝解剂,产物易分离。展开更多
The compound of tetraacetyldibenzylhexaazaisowurtzitane （TADBIW） is the precursor of synthesizing the high energy density caged compound hexanitrohexaazaisowurtzitane （HNIW）. TADBIW was obtained by hydrogenolysis ...The compound of tetraacetyldibenzylhexaazaisowurtzitane （TADBIW） is the precursor of synthesizing the high energy density caged compound hexanitrohexaazaisowurtzitane （HNIW）. TADBIW was obtained by hydrogenolysis of hexabenzylhexaazaisowurtzitane （HBIW）. The hydrogenolysis product TADBIW contains a little amount of triacetyltribenzylhexaazaisowurzitane （TATBIW）. It was proposed that the hydrogenolysis of HBIW would occur in a stepwise manner Two compounds, diacetyltetrabenzylhexaazaisowurtzitance （DATBIW） TATBIW, were synthesized by controlling the volumes of hydrogen that consumed during the hydrogenolysis debenzylation of HBIW. They are the intermediates of the hydrogenolysis of HBIW. The success of synthesizing these intermediates would be useful for researching the mechanism of the hydrogenolysis of HBIW. This is also useful for improving the hydrogenolysis process： increasing the amount of catalyst and prolonging the hours of reaction would produce high yields and enhance the purity of TADBIW.展开更多
文摘以四乙酰基二苄基六氮杂异伍兹烷为基质,经亚硝解脱苄合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW);用纯硝酸氧化TADNSIW制备四乙酰基二硝基六氮杂异伍兹烷(TADNIW),收率93.0%,以上两步反应均在室温下完成。在85℃条件下,TADNIW经硝硫混酸硝解合成了六硝基六氮杂异伍兹烷(HNIW),反应时间50 m in,收率95.1%,质量分数98.80%。用硝硫混酸对TADNSIW进行硝解合成了HNIW,并优化了反应条件,反应温度90℃,反应时间60 m in,硝解剂必须大于14 mL(底物TADNSIW 1.2 g),收率为96.1%,质量分数98.87%。分别用FTIR,1HNMR和元素分析对目标化合物进行了表征。前体TADNSIW和TADNIW分子中只有乙酰基和亚硝基,它们的硝解反应体系较简单,反应时间短、反应条件温和,母液中只含有乙酸和硝解剂,产物易分离。
文摘The compound of tetraacetyldibenzylhexaazaisowurtzitane （TADBIW） is the precursor of synthesizing the high energy density caged compound hexanitrohexaazaisowurtzitane （HNIW）. TADBIW was obtained by hydrogenolysis of hexabenzylhexaazaisowurtzitane （HBIW）. The hydrogenolysis product TADBIW contains a little amount of triacetyltribenzylhexaazaisowurzitane （TATBIW）. It was proposed that the hydrogenolysis of HBIW would occur in a stepwise manner Two compounds, diacetyltetrabenzylhexaazaisowurtzitance （DATBIW） TATBIW, were synthesized by controlling the volumes of hydrogen that consumed during the hydrogenolysis debenzylation of HBIW. They are the intermediates of the hydrogenolysis of HBIW. The success of synthesizing these intermediates would be useful for researching the mechanism of the hydrogenolysis of HBIW. This is also useful for improving the hydrogenolysis process： increasing the amount of catalyst and prolonging the hours of reaction would produce high yields and enhance the purity of TADBIW.
