2,2'-二甲基-1,1'-联二蒽醌合成工艺的优化

Synthesis Optimization of the 2,2'-Ddmethyl-1,1'-Dianthraquinonyl

以邻苯二甲酸酐和甲苯为原料,三氯化铝为催化剂,以发烟硫酸为闭环剂,二氯乙烷为介质,闭环生成2-甲基蒽醌;在活化铜粉为催化剂,以萘为溶剂下脱氯缩合制得2,2'-二甲基-1,1'-联二蒽醌,并对合成工艺进行了优化。优化条件为:采用分步法,制取2-甲基蒽醌,以萘为溶剂,n铜粉∶n1-氯-2-甲基蒽醌=1,反应温度230℃,保温3 h,在此条件下,目标产收率比原工艺提高10%。采用熔点测定、红外光谱(IR)、液相色谱(HLPC)进行分析和结构表征。

Phthalic anhydride and two toluene as raw material,aluminium trichloride as catalyst,fuming sulfuric acid as closed-loop agent,and dichloroethane as medium,closed loop generation 2-Methyl anthraquinone was synthesized.In the activation of copper powder as catalyst,naphthalene as solvent,under the dechlorination of condensation of 2,2＇-Dimethyl-1,1＇-Dianthraquinonyl,the synthesis process was optimized.Using the step-by-step method,2-Methyl anthraquinone was prepared,with naphthalene as solvent,copper powder and 1-chloro-2-methyl anthraquinone molar ratio 1：1,reaction temperature 230 ℃,and thermal insulation 3 h.On this condition,the target product yield increased by 10% than the original technology.Analysis and structure characterization of this produced were carried out with melting point,infrared spectroscopy（IR）,and liquid chromatography（HLPC）.