摘要
以2,6-二氨基吡啶为原料,经酰化、硝化反应制得2,6-二氨基-3,5-二硝基吡啶。在硝化反应过程中,通过四因素三水平的正交实验找到的最佳工艺条件为:V(溶剂浓硫酸):V(发烟硫酸)为5.3:1,滴加发烟硝酸的温度范围为-5~0℃,反应温度为20℃,反应时间为5h。产品经高效液相色谱分析,其含量达99.00%以上,以2,6-二氨基吡啶计收率为94.13%。
The 2,6-diamino-3,5-dinitropyridine was synthesized form 2,6-diaminopyridine by acylating and nitrifying reaction.The optimum process conditions in the nitrifying process were found out through a orthogonal test with four factors and three levels,that were as follow:the volume ratio of solvent concentrated sulfuric acid and oleum is 5.3:1,and the temperature range of dripping nitric acid is -5~0℃,reaction temperature is about 20℃,reaction time is 5 hours.A yield of about 94.13%and the purity to more than 99.00%were obtained.
出处
《精细与专用化学品》
CAS
2011年第1期36-39,共4页
Fine and Specialty Chemicals