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。
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.
出处
《林产化学与工业》
EI
CAS
CSCD
北大核心
2012年第2期71-74,共4页
Chemistry and Industry of Forest Products
基金
国家林业局948技术引进项目(2009-4-60)
