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以甲基环戊二烯(MCPD)为二烯体,马来酸酐(MA)为亲二烯体进行Dails-Alder(A-D)反应合成了甲基纳迪克酸酐(MNA)。考察了反应温度、反应时间、滴加温度、滴加时间及原料配比对产物收率的影响,并利用碘化学滴定法测定产物中外型反应物所占的比率,确定了适宜的合成条件:n(MA)∶n(MCPD)=0.8,反应温度为70℃,反应时间为100min,滴加温度为50℃,滴加时间为50min。产物的结构采用红外光谱和核磁共振谱进行分析。
Methyl nadic anhydride (MNA) was synthesized by Dails-Alder (A-D) reaction using methylcyclopentadiene (MCPD) as the diene and maleic anhydride (MA) as the dienophile. The effects of reaction temperature, reaction time, dropping temperature, dropping time and ratio of raw materials on the yield of the product were investigated. The ratio of external reactants in the product was determined by iodometric titration. The suitable synthesis conditions were determined: n (MA): n (MCPD) = 0.8, reaction temperature 70 ℃, reaction time 100min, dropping temperature 50 ℃, dropping time 50min. The structure of the product was analyzed by infrared spectroscopy and nuclear magnetic resonance spectroscopy.