绿色溶剂法制备2,6-二苦氨基吡啶的研究

Synthesis of 2,6-bis( picrylamino) pyridine in green solvent

采用水作为溶剂,以2,6-二氨基吡啶(DAP)和2,4,6-三硝基氯苯为原料,经N-烷基化反应,制得2,6-二苦氨基吡啶(PAP)。考察了相转移催化剂、反应物配比、缚酸剂用量、反应温度、反应时间等对PAP收率的影响。结果表明,优化工艺条件为:采用AEO9作相转移催化剂,n(三硝基氯苯)∶n(二氨基吡啶)=2.2∶1,n(碳酸氢钠)∶n(二氨基吡啶)=1.83∶1,反应温度95℃,反应时间为5 h。此时2,6-二苦氨基吡啶的得率可达84.6%,熔点315℃,液相色谱分析纯度为97.6%。

2,6-Bis（ picryl-amino） pyridine PAP was synthesis by 2,6-diaminopyridine and 2,4,6-nitrochlorobenzene in the real green solvent water. The effects of phase transfer catalyst,reactant proportion,acid-binding agent,reaction temperature and reaction time on the yield of PAP were researched. The result showed that the optimized reaction conditions of the condensation process were as following：AEO9 used as phase transfer catalyst,n（2,4,6-nitrochlorobenzene） ∶ n（2,6-diaminopyridine） = 2. 2 ∶ 1,n（ Na HCO3）∶ n（2,6-diaminopyridine） = 1. 83∶ 1,reaction temperature 95 ℃ and reaction time 5 h,with the yield of84. 6%,m. p. 315 ℃ and purity 97. 6% by high performance liquid chromatography.