医药中间体对氟苯丁酮的合成研究

在催化剂存在下,以对氟苯甲酸、丁酸为原料合成对氟苯丁酮,分别研究了缩合反应温度及反应时间、脱羧反应温度及反应时间、原料配比和催化剂用量等条件对合成对氟苯丁酮反应的影响,确定了最适宜的操作条件。该方法合成对氟苯丁酮的最佳操作条件是:缩合反应温度为165℃、缩合反应时间8.5h;脱羧反应温度为280～285℃、脱羧反应时间2.5h;n(丁酸):n(对氟苯甲酸)=0.7:0.1;催化剂还原铁粉的用量为2.5g(对氟苯甲酸为0.1mol的情况下)。对氟苯丁酮的收率可达到88.53%以上,产品纯度99.0%。

Study on Synthesis of p-Fluorobutyrophenone as a Medicine Intermediate

The catalytic synthesis of p-fluorobutyrophenone by the reaction of p-fluorobenzoic acid and nbutyric acid was studied.The effect of condensation reaction temperature,condensation reaction time, decarboxylation reaction temperature,decarboxylation reaction time,materials ratio and amount of catalyst on the synthesis was studied.The optimal reaction conditions were given as follows:condensation reaction temperature was 165℃,reaction time was 8.5 h,decarboxylation reaction temperature was 280～285℃,decarboxylation reaction time was 2.5 h,n(n-butyric acid):n(p-fluorobenzoic acid)=0.7:0.1, and the amount of iron catalyst was 2.5 g(when p-fluorobenzoic acid was 0.1 mol).The yield of p-fluorobutyrophenone reached 88.53%,and the purity of p-fluorobutyrophenone product was 99.0%.