亚甲基丁二酰氯的合成研究

摘要

以亚甲基丁二酸(衣康酸)为原料,采用五氯化磷为酰氯化试剂,通过熔融法合成了亚甲基丁二酰氯(衣康酰氯)。研究了反应物原料配比、反应时间、反应温度等因素对产物收率和纯度的影响,并且对产物的结构进行了红外光谱和核磁氢谱的表征。结果表明,在衣康酸和五氯化磷物质的量比为1∶2.2,温度110℃的条件下反应2 h,亚甲基丁二酰氯的收率可达到86%,纯度达到94%以上。%2-methylidenebutanedioyl dichloride (Itaconyl chloride ) was synthesized using itaconic acid and phosphorus pentachloride as raw materials by melting method.The effect of raw material ratio,reaction time,temperature and other process conditions on yield of product was examined.The structure of the product was characterized by IR and 1 H-NMR .The experiments showed that, when the itaconyl chloride and phosphorus pentachloride molar ratio was 1 ∶ 2.2, reaction temperature was 1 10 ℃ and reaction time was 2 h,the yield of 2-methylidenebutanedioyl dichloride can reach 86% and its purity was more than 94%.