【摘要】 缩酮经1,2-芳基转位重排催化反应合成3-氯-2,2-二甲基丙基布洛芬酯(布洛芬氯酯)是生产布洛芬的关键步骤。通过单因素实验考察了反应温度、催化剂浓度、催化剂滴加时间和反应时间对布洛芬氯酯收率的影响规律;结合响应面分析法对布洛芬氯酯合成工艺进行优化,确定了最佳工艺条件为反应温度136℃,催化剂浓度4.0%(质量分数),反应时间1.7 h,该工艺条件下产品收率预测值为97.78%,与实验值(97.72%)基本吻合;对催化剂失活原因进行了分析和验证,结果表明,原料液中含有的新戊二醇与催化剂发生反应,导致催化剂活性降低和反应速率变慢。更多还原

【Abstract】 The synthesis of 3-chloro-2,2-dimethylpropyl ester of ibuprofen(ibuprofen chloroester) from the ketal by 1,2-aryl-transposition rearrangement is a key step in the production of ibuprofen. The effects of reaction temperature, catalyst concentration, catalyst′s feeding time and reaction time on the yield of ibuprofen chloroester were investigated by single factor experiments. The response surface methodology was used to optimize the synthesis process of ibuprofen chloroester. The optimum conditions of this process were determined as follows: reaction temperature 136 ℃, mass fraction of catalyst 4.0% and reaction time 1.7 h. The predicted value of ibuprofen chloroester yield was 97.78% under the optimum conditions and was basically in agreement with the experimental value(97.72%). The reason for catalyst deactivation was analyzed and verified. The results showed that the neopentyl glycol contained in the raw material liquid reacted with the catalyst, which resulted in the reduction of the activity of the catalyst and the decrease of the reaction rate.更多还原