脱氢乙酸合成2,6-二甲基-γ-吡喃酮工艺研究  

2,6-Dimethyl-γ-pyranon synthetized by dehydroacetic acid

作　　者：陈秋云[1] 段正康[1] 彭叶[1] 李海涛[1] 颜志祥[1] 曾航日[1] 

机构地区：[1]湘潭大学化工学院绿色催化与反应工程湖南省普通高等学校重点实验室,湖南湘潭411105

出　　处：《化学试剂》2012年第10期941-945,共5页Chemical Reagents

基　　金：湖南省高校创新平台开放基金资助项目(11k062)

摘　　要：研究了脱氢乙酸制备标题化合物的合成方法与提取工艺。采用单因素试验考察了酸的种类与浓度、催化剂种类与用量、油浴温度与反应时间对反应产率的影响,得到的较佳工艺条件为:以杂多酸H4PW11VO40为催化剂、m(脱氢乙酸)∶m(H4PW11VO40)=5.5∶1,采用盐酸为反应介质、质量浓度为37.5%,油浴温度95℃,反应时间6 h,反应以脱氢乙酸计的产率为96.2%;对反应液进行了提取工艺研究,考察了萃取剂种类、溶液pH和盐析效应等对产物收率和含量的影响。采用HPLC分析了产物的纯度,其质量含量99%以上,收率85.4%,并利用红外光谱、核磁共振氢谱对产物的结构进行了表征。The synthesis method and extract process during preparation of 2, 6-dimethyl-γ-pyranon from dehydroacetic acid was researched. The effect of acid＇s type and concentra- tion,catalyst＇s type and the consumption, reaction time and reaction temperature on the yield was investigated by single factor experiments, and the optimized conditions were： H4 PW11 VO40 as catalyst, m （ dehydroacetic acid） ： m （ H4 PW11 VO460） = 5.5： 1, hydrochloric acid as reaction medium and the mass concentration was 37.5% ,oil bath temperature was 95 ℃ , reaction time was 6 h. The yield of 2,6-dimethyl-γ- pyranon could reach 96.2%. The extract process of reaction liquid was obtained,the effect of extractants＇ type,pH of liquid, salt effect,etc on the yield was investigated. The product was confirmed by FT-IR and ^1HNMR,the yield was 85.4% and its mass concentration was above 99%.

关 键 词：2 6-二甲基-γ-吡喃酮 脱氢乙酸 合成 分离提纯 

分 类 号：O621.3[理学—有机化学]