2,3-苯并环庚酮的合成

以苯和戊二酸酐为原料,经取代反应、沃夫-黄鸣龙还原和环化脱水,制得2,3-苯并环庚酮,最优反应条件为:n(戊二酸酐)∶n(苯)∶n(三氯化铝)=1∶2∶2,室温反应3 h,溶剂为四氢呋喃;沃夫-黄鸣龙还原反应温度为160℃,反应时间为2 h;环化脱水反应温度为120℃,时间2 h,反应总收率60.3%,用IR、1HNMR、13CNMR及MS对中间体及目标产物结构进行了表征。

Synthesis of 2, 3-Benzosuberone

2,3-Benzosuberone was synthesized using benzene and glutaric anhydride as raw materials through the Friedel-Crafts reaction,the Wolff-Huang-Minlon reduction and that cyclodehydration.Under the optimum reaction conditions of n(glutaric anhydride)∶n(benzene)∶n(AlCl3)=1∶2∶2,at room temperature for 3 h,and reduction at 160 ℃ for 2 h,then the cyclodehydration at 120 ℃ for 2 h.The overall yield was 60.3%.Structures of the intermediates and the final product were characterized by IR,NMR and MS.