4-(4-氯苯氧基)-2-氯苯乙酮的催化合成及微波促进作用

Catalytic Synthesis of 4-(4-Chlorophenoxy)- 2-chloroacetophenone and Microwave Promotion in the Reaction

系统研究了对氯苯酚与 2 ,4-二氯苯乙酮间的 Ullmann反应 ,考察了催化剂 ,反应溶剂 ,反应物配比 ,及微波辐射对反应的影响 .加入催化剂使反应的邻对位取代反应表现出很好的定位效应 .利用 GCD检测探讨了反应条件对反应副产物的影响 .研究表明 ,采用氯化亚铜为催化剂 ,以二甲苯与二甲基甲酰胺为混合溶剂 ,间二氯苯乙酮过量 2 0 %时能以较好的产率合成 4-(4 -氯苯氧基 ) -2 -氯苯乙酮 .微波辐射对

Ullmann reaction of p chlorophenol(Ⅹ) with 2,4 dichloroacetophenone(Ⅺ) was studied as functions of catalysts, solvent, reactants ratio and microwave irradiation. The reaction products were characterized by GC MS, 1H NMR and IR techniques. It is found that some catalysts have good regio selectivity for Ullmann reaction. With Cu 2Cl 2 as catalyst, AcNMe 2/Xylene as mixed solvent high yield of target compound was obtained. Microwave irradiation was found to accelerate the reaction.