(中南大學(xué) 化學(xué)化工學(xué)院，長(zhǎng)沙 410083)
摘 要: 以衣康酸和無水甲醇為原料，在酸性催化條件下酯化合成β-衣康酸單甲酯。研究催化劑種類與用量、物料配比、反應(yīng)溫度、反應(yīng)時(shí)間對(duì)β-衣康酸單甲酯收率的影響。得到的較佳合成工藝條件為：n(衣康酸)׃n(甲醇)׃n(苯甲酰氯)=1׃3.5׃0.043(摩爾比)，反應(yīng)溫度65 ℃，反應(yīng)時(shí)間30 min。粗產(chǎn)品用苯和石油醚的混合溶劑重結(jié)晶后，產(chǎn)物收率高達(dá)97.8%。采用FT-IR和1H-NMR對(duì)產(chǎn)物結(jié)構(gòu)進(jìn)行了表征。
關(guān)鍵字: 衣康酸；β-衣康酸甲酯；酯化；合成
（School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China）
Abstract:β-methylhydrogen itaconate was synthesized by using itaconic acid and methyl alcohol as raw materials and using acidic catalyst. The effects of kinds and quantity of catalysts, molar ratio of reactants, reaction time on the reaction were studied. The optimum conditions were obtained as follows: n(itaconic acid)׃n(methanol )׃n(benzoyl chloride)= 1׃3.5׃0.043 (molar ratio), reaction temperature 65 ℃, reaction time 30 min. The crude product was recrystallized from benzene and petroleum ether. Under above conditions, the yield of the product was 97.8%. The structure of the titled compound was determined by fourier-transferred infrared spectrum(FT-IR) and 1H-NMR.
Key words: itaconic acid; β-methylhydrogen itaconate; esterification; synthesis
