4-溴-4,4-二硝基丁酸乙酯的合成及表征

Synthesis and characterization of

摘要:

以溴代二硝基甲烷钾盐和丙烯酸乙酯为原料，在相转移催化剂四丁基溴化铵的作用下通过Michael 加成反应合成得到4-溴-4,4-二硝基丁酸乙酯。通过单因素方法，探讨了反应物料比、反应温度、反应时间及催化剂用量对产物产率的影响，得到该反应的最佳工艺条件为：反应温度为30 ℃，n(丙烯酸乙酯):n(溴代二硝基甲烷钾盐)为2:1，反应时间为30 min，四丁基溴化铵的用量为溴代二硝基甲烷钾盐质量的25%，产物产率可达到52%。同时用UV-Vis、FT-IR、1H NMR、MS以及元素分析等测试手段表征了产物的结构。

Abstract:

Ethyl 4-bromo-4,4-dinitrobutyrate was synthesized by Michael addition reaction of bromodinitromethane potassium salt and ethyl acrylate, and the effects of the ratio of raw materials, reaction temperature and time on the reaction were studied. The optimum synthetic technology conditions with 52% yield are: molar ratio 2:1 of ethyl acrylate to bromodinitromethane potassium salt, reaction temperature 30 ℃, reaction time 30 min, TBAB as phase transfer catalyst. The quality of TATB is equivalent to 25% of bromodinitromethane potassium salt. The structure of the product ethyl 4-bromo-4, 4-dinitrobutanoate was identified by IR, NMR, UV-Vis, MS and elementl analysis.