3,4-亚甲二氧基苯乙酮过氧酸氧化法合成芝麻酚  

Synthesis of 3,4-Methylenedioxyphenol by Acetylhydroperoxide Oxidation Method

作　　者：朱兆富[1] 沈喜海[1] 胡永利[1] 张志刚[1] 

机构地区：[1]河北职业技术师范学院化学系,河北昌黎066600

出　　处：《精细化工》2002年第11期667-668,671,共3页Fine Chemicals

摘　　要：3,4 亚甲二氧基苯乙酮 ,用过氧乙酸氧化生成乙酸 3,4 亚甲二氧基苯酚酯 ,此酯直接水解即获得产率 87 7%的芝麻酚 (3,4 亚甲二氧基苯酚 )。适宜的氧化条件 :n(过氧乙酸 )∶n(3,4 亚甲二氧基苯乙酮 ) =(1 0 5～ 1 15 )∶1,2 0～ 30℃反应 4h ,少量锌粉脱色 ;适宜的水解条件 :w(NaOH) =5 %水溶液室温反应 4h。3,4-Methylenedioxyphenol(Ⅰ)was prepared from 3,4 methylenedioxyacetophenone(Ⅱ)by oxidation with acetylhydroperoxide and hydrolysis.Effects of reaction conditions on yield and quality of the product were investigated. The optimum conditions of oxidation were n (CH 3COOH)∶ n (Ⅱ)=(1 05-1 15)∶1,reaction temperature 20-30 ℃ and reaction time 4 h.The crude acetic ester of Ⅰ was directly hydrolyzed with w (NaOH)=5% aqueous solution at room temperature for 4 h to give pure Ⅰ in 87 7% yield.

关 键 词：芝麻酚 3 4-亚甲二氧基苯乙酮 过氧乙酸 Baeyer-Villiger氧化反应 

分 类 号：TQ243.12[化学工程—有机化工]