【摘要】 以甲苯、氯苯、醋酸酐和苯甲酸乙酯为原料,先经傅克反应酰基化合成对甲基(氯)苯乙酮,再经克莱森酯缩合反应合成4-甲基(氯)二苯甲酰甲烷。用单因素实验法研究了缩合反应的各种影响因素,得到较佳工艺条件:甲苯为溶剂,氨基钠为缩合反应催化剂,微波辐射功率320 W,辐射时间45min,n(对甲基苯乙酮)∶n(苯甲酸乙酯)∶n(氨基钠)=1∶4∶5,4-甲基二苯甲酰甲烷收率72.2%;n(对氯苯乙酮)∶n(苯甲酸乙酯)∶n(氨基钠)=1∶2∶4;4-氯二苯甲酰甲烷收率83.3%。合成的产物经元素分析、IR与1 H NMR进行了结构表征,对UV光谱有良好的吸收,六个苯环上取代的二苯甲酰甲烷对猪油有较好的抗氧化作用。更多还原

【Abstract】 Methyl(chloro)-dibenzoylmethane was synthesized from toluene,chlorobenzene,acetic anhydride and benzoic acid ethyl ester via Friedel-Crafts acylation of methylacetophenone(chloroacetophenone)and subsequent Claisen condensation.Conditions influencing the result of Claisen condensation were investigated by single factor tests.Experimental results showed the suitable conditions are as follows:using toluene as solvent and sodium amide as catalyst,power of microwave irradiation of 320W,microwave irradiation time of 45min,and molar ratio of n(methyl acetophenone)∶n(benzonic acid ethyl ester)∶n(sodium amide)= 1∶4∶5.The yield of 4-methyl-dibenzoylmethane achieved 72.2%.When n(chloro acetophenone)∶n(benzonic acid ethyl ester)∶n(sodium amide)= 1∶2∶4,the yield of 4-chlorodibenzoylmethane achieved 83.3%.The structures of the products were characterized by elemental analysis,IR and 1H NMR.The products are good ultraviolet absorbents and exhibit significant antioxidation activity for lard.更多还原