含能材料
含能材料
함능재료
ENERGETIC MATERIALS
2014年
5期
722-724
,共3页
金兴辉%胡炳成%刘祖亮%吕春绪
金興輝%鬍炳成%劉祖亮%呂春緒
금흥휘%호병성%류조량%려춘서
有机化学%一锅法合成%4-硝基咪唑%硝化%2,4,5-三硝基咪唑
有機化學%一鍋法閤成%4-硝基咪唑%硝化%2,4,5-三硝基咪唑
유궤화학%일과법합성%4-초기미서%초화%2,4,5-삼초기미서
organic chemistry%one-pot synthesis%4-nitroimidazole%nitration%2,4,5-trinitroimidazole
以4-硝基咪唑为原料,用 HNO3/KI /AcOH 作为硝化体系,通过一锅法制备了2,4,5-三硝基咪唑,用1 H NMR,IR,MS 以及元素分析对其结构进行了表征。优化了反应路线,结果表明,在反应时间4 h,反应温度为120℃,n(4-硝基咪唑)∶ n(65%HNO3)∶ n(AcOH)=1∶30∶30条件下,目标化合物产率高达80.6%。
以4-硝基咪唑為原料,用 HNO3/KI /AcOH 作為硝化體繫,通過一鍋法製備瞭2,4,5-三硝基咪唑,用1 H NMR,IR,MS 以及元素分析對其結構進行瞭錶徵。優化瞭反應路線,結果錶明,在反應時間4 h,反應溫度為120℃,n(4-硝基咪唑)∶ n(65%HNO3)∶ n(AcOH)=1∶30∶30條件下,目標化閤物產率高達80.6%。
이4-초기미서위원료,용 HNO3/KI /AcOH 작위초화체계,통과일과법제비료2,4,5-삼초기미서,용1 H NMR,IR,MS 이급원소분석대기결구진행료표정。우화료반응로선,결과표명,재반응시간4 h,반응온도위120℃,n(4-초기미서)∶ n(65%HNO3)∶ n(AcOH)=1∶30∶30조건하,목표화합물산솔고체80.6%。
An improved one-pot method for the preparation of 2,4,5-trinitroimidazole from 4-nitroimidazole was reported. Its structure was identified by 1 H NMR,IR,MS and elemental analysis. The reaction time,reaction temperature and the molar ratio of the reagents of the synthetic route were optimized. Results show that the yield of 2,4,5-trinitroimidazole can reach up to 80. 6% under the conditions of reaction time 4 h,reaction tempera-ture 120 ℃ and the molar ratio of n(4-nitroimidazole)∶ n(65% HNO3 )∶ n( AcOH)= 1 ∶ 30 ∶ 30.