2,6-二苦胺基吡啶合成工艺优化研究

Studies on the synthesis of the 2,6-bis(picrylamino)pyridine

本研究以NaHCO_3为缚酸剂,工业乙醇为溶剂,三硝基氯苯和二氨基吡啶为原料合成2,6-二苦胺基吡啶、分别测试了三硝基氯苯与二氨基吡啶的物质的量之比,NaHCO_3的用量,反应时间,反应温度等因素对产物收率的影响。实验结果表明:在固定二氮基吡啶用量为0.41g的情况下,n(三硝基氯苯):n(二氨基吡啶)=2.2:1,NaHCO_3的用量为0.74g,反应温度为76℃,反应时间3小时的条件下,产品收率可大于93%。

In this paper,2,6-bis(picrylamino)pyridine was synthesized from trinitrochlorobenzene and diaminopyridine in the presence of the acid-binding agent NaHCO_3 and the solvent industrial ethanol.The factors influencing the yield of product are the molar ratio of trinitrochlorobenzene to diaminopyridine and the amount of NaHCO_3 and the reaction time and reaction temperature and so on,which were discussed.Experimental results showed that:under the condition of the amount of diamino pyridine is 0.41 g,the molar ratio of trinitrochlorobenzene to diaminopyridine is 2.2:1,the mass ratio of NaHCO_3 is 0.74 g,and the reaction temperature is 76℃ and the reaction time is 3 hours,the yield of product is more than 93%.