【摘要】 以Ullman反应为依据,采用工业上广泛使用的低毒二甲苯做溶剂,以铜粉做催化剂,乙酸钾做缚酸剂,通过1,5-二氯蒽醌与邻甲氧基苯胺的多相反应合成了1,5-双(邻甲氧基苯胺基)蒽醌,并详细考查了溶剂用量、催化剂用量、物料配比及反应时间等对反应的影响.发现在n(C14H6Cl2O2)∶n(C7H9NO)∶n(CH3COOK)=1∶10∶2.5,V(C8H10,mL)/m(C14H6Cl2O2,g)=18,w(Cu)=5.3%,回流10 h的条件下,1,5-二氯蒽醌的转化率为97.8%,产物1,5-双(邻甲氧基苯胺基)蒽醌的产率为80.6%,溶剂回收率为86%.产物经MS、1H NMR、IR及DSC分析证明结构正确.更多还原

【Abstract】 Based on the Ullman reaction mechanism,the synthesis of 1,5-di(o-anisidino) anthraquinone was achieved by the multiphase reaction of 1,5-dichloroanthraquinone in xylene and o-anisidine in the presence of Cu and potassium acetate.The effects of various factors on the reaction,such as the xylene dosage,catalyst dosage,molar ratio of raw materials,reaction time were determined.The conversion of 1,5-dichloroanthraquinone is 97.8% and the yield of 1,5-di(o-anisidino) anthraquinone is 80.6%,while the molar ratio of 1,5-dichloroanthraquinone to o-anisidine and potassium acetate is 1∶10∶2.5,V(C8H10,mL)/m(C14H6Cl2O2,g)=18,the catalyst dosage based on 1,5-dichloroanthraquinone is 5.3%,and the mixture is refluxed for 10 h.Under these conditions,the recovery of the solvent is 86%.The target compound was identified by MS,1H NMR,IR and DSC.更多还原