火炸药学报2017，Vol.40Issue(5)：45-50,6.DOI:10.14077/j.issn.1007-7812.2017.05.008
3,3'-双(2,2-二甲基-5-硝基-1,3-二氧杂环己烷-5-ONN-氧化偶氮基)氧化偶氮呋咱(BDDAF)的合成、晶体结构与热行为
Synthesis, Crystal Structure and Thermal Behavior of 3,3'-Bis(2,2-dimethyl-5-nitro-1,3-dioxan-5-yl-ONN-azoxy) azoxyfurazan (BDDAF)
摘要
Abstract
Taking tri(hydroxymethyl) nitromethane (TN) and acetone as raw materials,2,2-dimethyl-5-nitro-5-nitroso 1,3-dioxane(DMNNDO) was synthesized via.condensation,alkaline hydrolysis and nitrosation reactions.The energetic intermediate 3,3'-bis (2,2-dimethyl-5-nitro-1,3-dioxan-5-yl-ONN-azoxy) azoxyfurazan (BDDAF) was synthesized via.oxidative-coupling reaction taking DMNNDO and DAOAF as starting materials,and the total yield of this four-step reactions was 40％.The structure of target compound was characterized by IR,1H NMR,13C NMR,15 N NMR and elemental analysis.The single crystal of BDDAF was cultured and its structure was characterized by X-ray single crystal diffractometer.The thermal behavior of BDDAF was investigated by differential scanning calorimetry(DSC) and thermogravimetric analysis (TG) method.The results show that the crystal belongs to monoclinic system,space group is P2(1)/n,cell parameters are a=0.54504(15)nm,b=3.1462(9),c=0.7546(2),β =103.612(5)°,V=1.257 7(6)nm3,Z=2,Dc=1.554g/cm3,F(000)=608,ωR1 =0.1387 and ωR2 =0.3306.The oxidative coupling reaction conditions are optimized and the yield can reach 85 ％.The solvent-nonsolvent method is used instead of column chromatography,the purity of BDDAF is more than 99 ％,and the melting point and decomposition temperature are 117℃ and 248℃,respectively.关键词
有机化学/三羟甲基硝基甲烷/氧化偶氮呋咱/含能化合物/BDDAFKey words
organic chemistry/tri(hydroxymethyl) nitromethane/azoxy frazan/energetic compounds/BDDAF分类
军事科技引用本文复制引用
张家荣,毕福强,王伯周,张俊林,贾思媛..3,3'-双(2,2-二甲基-5-硝基-1,3-二氧杂环己烷-5-ONN-氧化偶氮基)氧化偶氮呋咱(BDDAF)的合成、晶体结构与热行为[J].火炸药学报,2017,40(5):45-50,6.基金项目
国家自然科学基金资助(No.21243007) （No.21243007）
