文章改进了合成方法并合成新型非对称酞菁.非对称酞菁是以4-(对叔丁基苯氧基)邻苯二腈(A)、1,3-二亚胺基异吲哚啉(B)和二水乙酸合锰作为起始原料合成的.合成方法简述如下:原料在有机溶剂正戊醇中加热搅拌,加入适量的催化剂1,8-二氮杂-双环(5,4,O)十一碳烯-7(DBU)进行反应.反应完毕后,冷却至室温,向反应物中加入无水甲醇,析出固体,减压除去溶剂.首先产物用甲醇在索氏提取器中索提12h,最后得到目标化合物.非对称酞菁经过红外、原子吸收紫外可见光谱和元素分析表征证明其结构,从而证实产物就是目标化合物.
A new unsymmetry phthalocyanine was synthesized through an improved synthetic method.A mixture of 4-(p-tert-butylphenoxy)phthalonitrile(A),1,3-diiminoisoindoline(B) and Mn(AcO)2·2H2O was added to organic solvent [1-pentanol] under stirring.Then,the suitable catalyst of 1,8-diazabicyclo [5,4,0]undec-7-ene(DBU) was added,and the mixture was heated under N2 for over 12 h.After cooling,anhydrous methanol was added into the reaction mixture to obtain the solid.The solvent was removed under reduced pressure.The collected solid powder was extracted with anhydrous methanol in a soxhlet extractor for 24 h and further purified twice by chromatography.The obtained unsymmetry substituted phthalocyanine was characterized by ultraviolet-visible spectroscopy(UV/Vis),infrared spectroscopy(IR),atomic absorption spectroscopy and elemental analysis.The results are in agreement with the proposed structures.