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CN101696198A 2,5-二甲基-4-羟基-3(2H)呋喃酮的制备方法 有权 转让

2,5-二甲基-4-羟基-3(2H)呋喃酮的制备方法
摘要：
2，5-二甲基-4-羟基-3(2H)呋喃酮的制备方法。以3，4-己二酮为原料，10～25℃无需溶剂滴加溴素5-6h，发生取代反应，保温反应3-6h，经过中和、真空蒸馏得到的2，5-二溴-3，4-己二酮，收率70-90％。继而用2，5-二溴-3，4-己二酮在碱金属盐作用下60-90℃水解反应6-12h，经过中和、洗涤、萃取、浓缩、结晶、重结晶得产品2，5-二甲基-4-羟基-3-(2H)呋喃酮，收率50-60％，熔点75-78℃，含量为＞98％。本发明与现有技术相比，操作简单，收率高，降低生产成本。
摘要（英）：

The invention discloses a preparation method of 2,5-dimethyl-4-oxhydryl-3(2H) furanone, comprising the following steps of: dropping bromine at 0-25 DEG C for 5-6h without adding a solvent by taking 3,4-hexanedione as raw materials, undergoing substitution reaction, reacting for 3-6h by keeping the temperature, and then neutralizing and distilling in vacuum to obtain 2,5-dibromo-3,4-hexanedione with the yield of 70-90 percent; afterwards, carrying out hydrolysis reaction on the 2,5-dibromo-3,4-hexanedione under the action of an alkali metal salt at 60-90 DEG C for 6-12h, and then neutralizing, washing, extracting, concentrating, crystallizing and recrystallizing to obtain the 2,5-dimethyl-4-oxhydryl-3(2H) furanone with the yield of 50-60 percent, the melting point of 75-78 DEG C and the content of more than 98 percent. Compared with the prior art, the invention has the advantages of simple operation, high yield and production cost reduction.

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