2-甲氧基-4'-三氟甲基苯乙酮的合成

Synthesis of 2-Methoxy-4'-trifluoromethyl Acetophenone

以4-三氟甲基苯甲酸甲酯和甲氧基乙酸甲酯为原料,在碱性条件下进行交叉酯缩合反应,然后经水解、脱羧得到产品2-甲氧基-4'-三氟甲基苯乙酮,总收率达85%以上。实验获得了较佳工艺条件:原料配比4-三氟甲基苯甲酸甲酯/甲氧基乙酸甲酯为1/1.5(mol/mol),酯缩合的反应温度为30℃、反应时间为12h,适宜的溶剂为DMSO;水解、脱羧反应时间为15h;并采用1HNMR及IR对产品进行了表征。

A new method was proposed to prepare 2-methoxy-4'-trifluoromethyl acetophenone with higher yield and simpler operation conditions. Starting from methyl 4-trifluoromethyl benzoate (TFMB) and methyl methoxyacetate (MTA), the title compound was prepared via cross ester condensation, hydrolysis and decarboxylation with overall yield higher than 85%. The effects of reaction time, temperature, feeds molar ratio and solvent on the conversion of ester condensation were investigated, and the optimum reaction conditions were obtained as following: TFMB/MTA 1/1.5 (molar ratio), the cross ester condensation time 12 h, the hydrolysis and decarboxylation time 15 h; the cross ester condensation temperature 30°C, and the suitable solvent for this condensation reaction is dimethyl sulfoxide (DMSO).