摘要
[目的]探讨合成3-乙氧基-4-乙氧羰基苯乙酸的方法。[方法]4-甲基水杨酸经溴乙烷烷基化得到2-乙氧基-4-甲基苯甲酸乙酯,再在二异丙胺锂(LDA),六甲基磷酰胺(HMPA)和CO2共同作用下在苄位进行羧基化得到目标产物。[结果]得到27 g白色粉末状终产物,熔点74~76℃,产率为73%,经1H NMR和MS鉴定为3-乙氧基-4-乙氧羰基苯乙酸。[结论]该合成方法路线较短,操作简单,易于纯化,适合于工业化生产。
[Objective] To study a method to synthesize 3-ethoxy-4-ethoxy-carbonyl-phenylacetic acid.[Method] 4-Methylsalicylic acid was alkylated to produce 2-hydroxy-4-methylbenzoic acid ester,which was then carboxylated by lithium diisopropylamide(LDA),Hexamethyl phosphoryl triamide(HMPA) and CO2,to obtain the final products.[Result] The final products of 27 g white powders was identified by 1H NMR and MS to be 3-ethoxy-4-ethoxy-carbonyl-phenylacetic acid,whose melting point was 74-76 ℃ and yield was 73%.[Conclusion] The synthesis method was simple,convenient and applicable to industrial production.
出处
《安徽农业科学》
CAS
北大核心
2011年第29期17907-17908,17919,共3页
Journal of Anhui Agricultural Sciences
基金
四川省教育厅自然科学青年项目(11205023)
西华大学重点科研基金项目(Z1020519)