DBU催化去甲氨噻肟乙酯三苯甲基化反应的研究

Study on Triphenyl Methylation of Demethylaminothiaoxime Ethyl Sster Catalyzed by DBU

以1,8-二氮杂二环十一碳-7-烯(DBU)为催化剂,三苯氯甲烷为三苯甲基化试剂,研究了去甲氨噻肟乙酯的三苯甲基化反应。分析了反应机理,筛选了催化剂,考察了溶剂、反应温度、反应时间及摩尔配比等因素对实验结果的影响,得到了较佳的合成工艺。以四氢呋喃为溶剂,反应物摩尔比为1∶1.1,反应温度为40℃,反应时间为4h时,总收率可达到82.3%。对比了DBU和传统催化剂的优劣,可为工业化生产头孢地尼提供技术参考。

Applied 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) as catalyst, tribenzene chloromethane as tribenzene methylation re-agent, the tribenzene methylation reaction of demethylamphetamine was studied. The reaction mechanism was analyzed, the effects of solvent, reaction temperature, reaction time and molar ratio on the experimental results were investigated, and a better synthesis process was obtained. When the tetrahydrofuran as the solvent, the reactor molar ratio was 1:1, the reaction temperature was 40℃ , the reaction time was 4h, the total yield could reach 82.3%. At the same time, the advantages and disadvantages of DBU and tradi-tional catalysts were compared in order to provide technical reference for the industrial production of cephalosporine.