邻羟基苯丁酮的合成工艺研究

以丁酸苯酯为原料,三氯化铝作催化剂,在硝基苯溶剂中经Fries重排反应制备了邻/对羟基苯丁酮。反应体系采用气相色谱进行定量分析。通过单因素实验和正交实验考察了反应时间、催化剂用量及反应温度对邻/对羟基苯丁酮收率的影响,确定了优化工艺条件。实验结果表明,当反应温度为120℃、n(催化剂)∶n(丁酸苯酯)=1.6∶1、反应时间2 h时,丁酸苯酯完全转化,反应总收率大于80%,其中邻羟基苯丁酮收率大于48%。

Study on the Synthesis of o-Hydroxybutyrophenone

o/p-Hydroxybutyrophenone（o / p-HBP） was prepared from phenyl butyrate（PB） in nitrobenzene via Fries rearrangement in the presence of AlCl3.The influences of reaction time,catalyst dosage and reaction temperature on the yield of o/p-HBP were discussed based on single-factor experiments and orthogonal experiments.Under optimal conditions（120℃ / 2 h,n（cat）∶n（PB）=1.6） the product mixture was formed in 80% yield,of which 60% was o-HBP.