响应面优化食品添加剂中间体2-甲基-2-仲丁基丙二酸二乙酯合成工艺

Optimization of Synthesis Process for 2-Methyl-2-Sec-Butyl Malonate for Use as a Synthetic Intermediate of Food Additives

以甲基丙二酸二乙酯和2-溴丁烷为原料、乙醇钠为催化剂,经烷基化反应合成了食品增香剂中间体2-甲基-2-仲丁基丙二酸二乙酯。对影响产率的原料物质的量比、反应时间、反应温度和催化剂等单因素水平考察的基础上,应用响应面分析法进行了工艺优化。通过气相色谱和核磁波谱数据分析确证了2-甲基-2-仲丁基丙二酸二乙酯的结构。其工艺简单、操作简便、原料易得、反应条件较温和、产品易于分离且成本低。反应最终产率平均值为(70.6±0.11)%,具有工业化应用前景。

The synthesis of 2-methyl-2-sec-butyl malonate as a synthetic intermediate of food flavoring agents via the alkylation reaction of diethyl methylmalonate with 2-bromobutane catalyzed by sodium ethoxide was optimized by the combined use of single factor method and response surface methodology. The yield of 2-methyl-2-sec-butyl malonate was investigated with respect to ratio of diethyl methylmalonate to sodium, ratio of diethyl methylmalonate to 2-bromobutane, reaction time and temperature. The synthetic 2-methyl-2-sec-butyl malonate was structurally characterized by gas chromatography(GC) and nuclear magnetic resonance(NMR) spectroscopy. The synthesis procedure presented in this study was simple, easy to operate and economical and could produce easy-to-separate products from easily available materials under mild reaction conditions. With this procedure, the average yield of the final product was(70.6 ± 0.11)%. In conclusion, it has promising prospects for industrial application.