摘要
以3,4-二氨基呋咱(DAF)为原料,经Caro-acid氧化生成二硝基呋咱(DNF),碱性条件下DNF分子间硝基醚化后合成目标化合物4,4′-二硝基双呋咱醚(FOF-1)。采用红外光谱、质谱、元素分析及核磁共振进行了结构表征;初步探讨了硝基分子间醚化合成FOF-1的反应机理;优化了氧化、分子间醚化工艺,确定了最佳合成条件:氧化反应时间为3.5h,H2SO4的起始浓度为51.7%,醚化反应时间为2.5h,水质量分数小于0.03%。总收率达到42%,纯度为99.6%。
4,4＇-Dinitrodifurazalyl ether（FOF-1）was synthesized from 3,4 diamino-furazan （DAF） after Caro acid oxidation and etherification of nitro-group. Its structure was characterized by IR, MS, NMR and elemental analysis. The reaction mechanism of intermolecular etherification of nitro group was preliminarily discussed. In addition, the synthetic procedures were optimized, and the optimal conditions of oxidization and intermolecular etherification reaction were determined. The best condition was obtained as follows ： the oxidation reaction time is 3. 5h, initial content of H2SO4 is 51. 7%, the etherification reaction time is 2.5h, content of water is less tan 0.03%, the overall yields is 42% and the purity is 99.6%.
出处
《火炸药学报》
EI
CAS
CSCD
2008年第5期12-14,27,共4页
Chinese Journal of Explosives & Propellants
