1,3-双(4-氨基苯氧基)苯的合成方法研究

Study on synthetic method of 1,3-bis(4-aminophenoxy)benzene

间苯二酚和对氯硝基苯经缩合反应、合成得到1,3-双(4-硝基苯氧基)苯,以FeCl3.6H2O/C为催化剂,水合肼为还原剂,在乙醇中还原得到1,3-双(4-氨基苯氧基)苯。采用薄层色谱(TLC)对反应进程进行了跟踪研究,并用熔点测定仪、DSC,FT-IR、1H-NMR和元素分析等分析方法对目标产物的结构进行了表征。试验结果表明:当m[1,3-双(4-硝基苯氧基)苯]=14.1 g(40.1 mmol)、V(水合肼)=20 mL时,选择催化剂m(FeCl3.6H2O)=1.00 g、m(C)=2.50 g进行反应,并控制水合肼加入时的反应温度为70℃,加完以后在回流温度进行反应,还原反应产物的得率可达60%左右[以1,3-双(4-硝基苯氧基)苯计]。

The 1,3-bis （4-nitrophenoxy）benzene was synthesized from the condensation reaction of resorcinol with 4-nitroehlorobenzene. The 1,3-bis（4-aminophenoxy） benzene was prepared from the reduction reaction of 1,3-bis（4-nitrophenoxy） benzene in ethanol solvent with FeCl3·6H2O and C as catalyst,the hydrazine hydrate as reducing agent,and the reaction progress was tracked and studied by thin-layer chromatography（TLC） method, and the structure of target produce was characterized by melting point apparatus, DSC, FT-IR, IH-NMR spectra and elemental analysis etc. ways. The testing results showed when the mass of 1,3-bis（4-nitrophenoxy） benzene was 14.1 g（40.1 mmol） ,and the volume fraction of hydrazine hydrate was 20 mL,selected the catalyst FeCl3·6H2O＇s mass was 1.00 g, and active carbon ＇.s mass was 2.50 g,and control reaction temperature of added the hydrazine hydrate was 70 ℃, after added finish,the reaction mixture was agitated and maintained at the refluence temperature, the yield of 1,3-bis （4-aminophenoxy） benzene was about 60% （according to the 1,3-bis （4-nitrophenoxy） benzene）.