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4,6-二羟基苯-4’-羟基苯乙酮的合成研究
Synthesis of 4,6-Dihydroxybenzene-4’-Hydroxyacetophenone
【摘要】 4,6-二羟基苯-4’-羟基苯乙酮是制备大豆苷元的关键中间体。以间苯二酚和对羟基苯乙酸为原料经傅克酰基化反应生成目标产物。采用路易斯酸催化剂三氟甲磺酸锌代替三氟化硼乙醚,解决了处理过程中的废水问题;探讨了催化剂种类、催化剂摩尔分数、反应温度与时间等条件的影响;最优条件为:n(间苯二酚)∶n(对羟基苯乙酸)=1∶1,在120℃熔融状态反应10 h,添加摩尔分数8.25%三氟甲磺酸锌作为催化剂。在最优条件下总产率可达到50.4%,解决了现有工艺三氟化硼乙醚作催化剂腐蚀玻璃反应釜的问题。
【Abstract】 4,6-Dihydroxybenzene-4’-hydroxyacetophenone is a key intermediate for the preparation of daidzein. Using resorcinol and p-hydroxyphenylacetic acid as raw materials, the target product was prepared by Friedel-Crafts Acylation.The Lewis acid catalyst zinc trifluoromethanesulfonate was used instead of the traditional Lewis acid catalyst boron(tri)fluoride etherate to reduce the wastewater problem in the treatment process. The effects of catalyst type, catalyst mole fraction, reaction temperature and time on the reaction were discussed. The optimal conditions was as follows:n(resorcinol):n(p-hydroxyphenylacetic acid)= 1∶1, reaction temperature 120 ℃, molten state, reaction time 10 h,adding mole fraction 8.25% zinc trifluoromethanesulfonate as catalyst. Under above conditions, the total yield could reach 50.4%. The problem of using boron trifluoride ether as catalyst to corrode glass reactor was solved.
【Key words】 4,6-Dihydroxybenzene-4’-hydroxyacetophenone; Friedel-Crafts Acylation; Green chemistry; Catalytic reaction;
- 【文献出处】 当代化工 ,Contemporary Chemical Industry , 编辑部邮箱 ,2024年12期
- 【分类号】TQ244.2;O643.36
- 【下载频次】24