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Hoesch反应法合成2,3,4,4'-四羟基二苯甲酮的研究

Synthesis of 2,3,4,4'-tetrahydroxybenzophenone via Hoesch Reaction

  • 摘要: 提出了一种新颖的合成2,3,4,4'-四羟基二苯甲酮的方法。以焦性没食子酸和对羟基苯甲腈为原料,于无水乙醚中在氯化氢和Lewis酸ZnCl2存在下发生Hoesch反应,经后处理得到2,3,4,4'-四羟基二苯甲酮。通过正交试验对影响反应的因素进行了考察,确定了最优工艺条件:焦性没食子酸与对羟基苯甲腈的物质的量比为1:0.96,催化剂54.4 g(相对于1 mol焦性没食子酸),反应温度20 ℃,反应时间24 h。在此条件下产品得率达90 %以上,产品纯度在98 %以上。

     

    Abstract: A new synthetic approach to 2,3,4,4'-tetrahydroxybenzophenone was described. By means of pyrogallol and 4-cyanophenol as raw materials and diethyl ether as solvent, Hoesch reaction was carried out in the presence of HCl and ZnCl2 . Finally, 2,3,4,4'-tetrahydroxybenzophenone was synthesized. Influences of reaction were studied by orthogonal test method. The optimum process conditions were as follows: reaction material proportion of pyrogallol to 4-Cyanophenol 1:0.96(mol:mol),dosage of catalyzer 54.4 g(1 mol pyrogallol comparatively),reaction temperature 20 ℃ and reaction time 24 h.The yield of 2,3,4,4'-tetrahydroxybenzophenone was over 90 % and the product purity was over 98 % under this condition.

     

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