液质联用法用于5-氨基-1,10-邻菲罗啉的合成及工艺优化

Synthesis and Process Optimization of 5-Amino-1,10-Phenanthroline by Liquid Chromatography-Mass Spectrometry

以1,10-邻菲罗啉为起始原料合成了5-硝基-1,10~邻菲罗啉,产率为96.8%;进一步以氯化亚锡还原法合成了5-氨基-1,10-邻菲罗啉,考察了反应温度、反应时间和溶剂用量对还原反应的影响,并采用液质联用法监测反应,推断出可能的副反应,研究了氯化亚锡还原法的最佳反应条件,5-氨基-1.10-邻菲罗啉的产率由文献值10.1%提高到52.4%,纯度达99.0%。

5-Nitro-1, 10-phenanthroline was synthesized using 1,10-phenanthroline as starting material, and the yield was 96. 8%. 5-Amino-i, 10-phenanthroline was further synthesized by stannous chloride reduction method. Effects of reaction temperature, reaction time and solvent dosage on the reduction reaction were investi- gated. Liquid chromatography-mass spectrometry was applied to monitor the reaction. The possible side-reac- tions were deduced. The optimal reaction conditions of stannous chloride reduction method were also worked out. The yield of 5-amino-1, 10-phenanthroline increased from the reported 10. 1% to 52.4%, and the purity reached 99.0%.