2,4-二硝基苯磺酰胺的合成工艺改进

以2,4-二硝基苯胺为原料，依次经重氮化和磺化反应制得2,4-二硝基苯磺酰氯(3)； 3与氨水反应合成了2,4-二硝基苯磺酰胺(4)，其结构经¹H NMR, ¹³C NMR, EI-MS和元素分析确证。研究了反应时间，反应温度，溶剂，物料比{r［n(氨水):n(3)］}和加料次序对4收率的影响。结果表明：在最佳反应条件［THF为溶剂，氨水75 mmol, r=1.5，于10~30 ℃反应3 h］下合成4，收率91.3%。

Process Improvement on Synthesis of 2,4-Dinitrobenzenesulfonamide

2,4-Dinitrobenzene sulfonyl chloride (3) was prepared by diazotization and sulfonation , using 2,4-dinitroaniline as material .2,4-Dinitrobenzenesulfonamide (4) was synthesized by the reaction of 3 and ammonia .The structure was confirmed by 1 H NMR, 13 C NMR, EI-MS and elemental analysis . Effects of reaction time, reaction temperature, solvent, molar ratio{r[n(ammonia)∶n(3)]} and molar sequence on yield of 4 were investigated .The results indicated that the yield of 4 was 91.3%under the optimum condition[THF as solvent, ammonia 75 mmol, r=1.5, reacted at 10~30℃for 3 h].