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以布洛芬和甲醇为原料,以对甲苯磺酸为催化剂,以甘油作为吸水剂和催化剂分离的溶剂,利用甘油与布洛芬甲酯可自动分层的特性,辅以柱色谱分离,建立了一种布洛芬甲酯的绿色合成工艺。整个工艺路线无三废产生。合成条件经正交实验优化,确定了最佳反应条件:反应体系的最佳组成为n(布洛芬):n(甲醇):n(甘油)=1:10.2:1.4,催化剂对甲苯磺酸的最佳添加量为布洛芬质量的1%,最佳转速为300 r/min,最佳反应时间为4h,在该条件下转化率可达97.1%,得率大于95.0%。经液相-质谱联用(LC/MS)检测,色谱纯度为99.9%。
Using ibuprofen and methanol as raw materials, p-toluenesulfonic acid as catalyst and glycerol as water-absorbing agent and catalyst, the characteristics of glycerol and ibuprofen methyl ester can be automatically stratified, and combined with column chromatography to establish A green synthetic process of ibuprofen methyl ester. No waste generated throughout the process line. The optimal reaction conditions were determined by orthogonal experiment. The optimal reaction conditions were n (ibuprofen): n (methanol): n (glycerol) = 1: 10.2: 1.4 and the catalyst p-toluenesulfonic acid The best addition rate of ibuprofen was 1%, the optimum speed was 300 r / min, the best reaction time was 4h, the conversion rate was 97.1% and the yield was more than 95.0%. The liquid chromatography-mass spectrometry (LC / MS) detection, the chromatographic purity of 99.9%.