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以4,6-二氨基-1,3-苯二酚盐酸盐和对氨基苯甲酸为原料,在多聚磷酸介质中,合成2,6-二(4-氨基苯基)苯并[1,2-d;5,4-d’]二口恶唑,并利用红外光谱进行结构表征.考察反应温度、反应体系中P2O5质量分数、重结晶溶剂的选择以及还原剂SnCl2用量对产率的影响,得出最佳反应条件为:在氮气保护下,脱除HCl的最佳时间是18 h;多聚磷酸中w(P2O5)=82.5%;反应的最佳温度为200℃;重结晶试剂采用水;SnCl2用量为0.5 g时的产率最高,产率大于90%.
Using 2,6-bis (4-aminophenyl) benzo [1] as a starting material and 4,6-diamino-1,3-benzenediol and p-aminobenzoic acid as raw materials in a polyphosphoric acid medium , 2-d; 5,4-d ’] oxazoles were synthesized and characterized by FT-IR. The effects of reaction temperature, mass fraction of P2O5, choice of recrystallization solvent and amount of SnCl2 on yield The optimal reaction conditions were as follows: the best time for removing HCl under nitrogen was 18 h; the content of P (P2O5) in polyphosphoric acid was 82.5%; the optimal reaction temperature was 200 ℃; the recrystallization reagent Water; SnCl2 dosage of 0.5 g when the highest yield, yield greater than 90%.