5,7-二氨基-4,6-二硝基苯并氧化呋咱的制备

摘要

Using 2-Nitroaniline as the starting materials, the synthesis and refining of 5,7-diamino-4,6-dinitro-benzenfuroxan, 5,7-diamino-4,6-dinitrobenzenfuroxan was studied by the employment of a three step reaction, including oxidation, nitration and vicarious nucleophilic substitution (VNS) , having a total yield of 46%. The influencing factors of nitration reaction and vicarious nucleophilic substitution were studied, and the optimal reactive conditions were verified as follows; the optimal nitration temperature of 30℃ , the reactive time of vicarious nucleophilic substitution (VNS) of 3h, and the concentration of HC1 of 1 mol/L. Refining technology of DADNBF was designed as recrystallization of DADNBF potassium followed by acidizing, and the effect of recrystallization solvent on the purity and recrystallization yield was studied. Water was turned out to be the best solvent, the recrystallization yield was 92% , and the purity of DADNBF after acidizing was above 98. 8% . The product was characterized by1H NMR, MS and IR.%研究了5,7-二氨基4,6-二硝基苯并氧化呋咱(DADNBF)的合成与精制.以邻硝基苯胺为起始原料,经氧化、硝化、VNS胺化3步反应得到5,7-二氨基-4,6-二硝基苯并氧化呋咱,3步总收率46％,讨论了硝化反应和VNS胺化反应的影响因素,确定了合成DADNBF的最佳反应条件:适宜硝化温度为30℃,VNS胺化反应时间为3h,酸化使用盐酸的浓度为1 mol/L.设计了由DADNBF钾盐重结晶,再酸化制备DADNBF的精制工艺,研究了重结晶溶剂对DADNBF钾盐收率和纯度的影响,确定水为最佳溶剂,重结晶产率为92％,酸化后DADNBF的纯度≥98.8％.采用核磁共振、红外光谱、质谱对目标化合物的结构进行了表征.