3-甲基-2-氧代丁酸钠合成及表征

采用甲醇钠催化异丁醛与草酸二乙酯反应,一釜法合成了3-甲基-2-氧代丁酸钠。在反应料比单因素研究基础上,通过正交实验优化确定了最佳合成工艺条件,即:n(甲醇钠)∶n(异丁醛)∶n(氢氧化钠)∶n(甲醇)∶n(草酸二乙酯)=1.4∶1.4∶1.2∶7.5∶1,合成收率为75%。产品经熔点测定,IR、1H NMR1、3C NMR及元素分析,确认为预想结构,经HPLC分析确定纯度≥98%。

Synthesis and characterization for 3-methyl-2-oxobutanoic acid, sodium

By reacting isobutyraldehyde with diethyl oxalate using sodium methoxide as catalyst,3-methyl-2-oxobutanoic acid,sodium salt was prepared by one pot.On basis of investigating the single factor level of starting materials,the best synthetic process was determined through the orthogonal experiments,are that n(sodium methoxide) ∶n(isobutyraldehyde) ∶n(sodium hydroxide) ∶n(methanol) ∶n(diethyl oxalate) =1.4 ∶1.4 ∶1.2 ∶7.5 ∶1,and the yield can reach 75%.The data of element analysis,melting point,IR and NMR for the product are consistent with the standard data,the purity exceeds 98%.