2,6-二(4-氨基苯基)苯并[1,2-d;5,4-d']二口恶唑的合成

Synthesis of 2,6-bis(4-aminophenyl) benzo[1,2-d;5,4-d '] bisoxazole

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%.

2,6-bis（4-aminophenyl）benzo[1,2-d;5,4-d＇]bimxazole was synthesized in Italy （phosphoric acid） with 4,6-diamino-1,3-benzenediol dihydrochloride and p-aminobenzoic acid as materials. Its structure was determined by IR spectra. The effects of reacting temperature, the content of P2O5, recrystal lization agents and the content of SnCl2 on the yield of the product were analyzed. It was found that at the optimum reaction condition,the time of the dihydrochloride is 18 h in nitrogen, ω（P2O5）= 82.5 % ,the best reacting temperature is 200 ℃and the amount of SnC12 used in this paper is 0.5 g. The yield of the product obtained is above 90 %.