甲烷磺酸/氯化锌体系一步合成3,4,4’-三羟基二苯甲酮  

Synthesis of 3,4,4’-Trihydroxylbenzophenone in One Step by Methanesulfonic Acid/Zinc Chloride System

作　　者：邓方坤 危云云 张鹏[1] 翁雅青[1] 胡居吾[1] 刘栋 DENG Fangkun;WEI Yunyun;ZHANG Peng;WENG Yaqin;HU Juwu;LIU Dong(Institute of Applied Chemistry,Jiangxi Academy of Sciences,Nanchang 330096,China)

机构地区：[1]江西省科学院应用化学研究所,江西南昌330096

出　　处：《生物化工》2024年第5期61-64,70,共5页Biological Chemical Engineering

基　　金：江西省科学院省级财政科研项目(2022YSBG21022)。

摘　　要：多羟基二苯甲酮类化合物是一类广泛用作紫外线吸收剂的化合物。以苯酚、3,4-二羟基苯甲酸为原料,甲烷磺酸为溶剂,氯化锌为催化剂,一步合成了3,4,4’-三羟基二苯甲酮。通过试验考察了反应时间、反应温度、甲烷磺酸加入量、氯化锌加入量、后处理冰水用量对反应的影响。试验结果表明,3,4-二羟基苯甲酸0.1 mol,苯酚0.1 mol,甲烷磺酸1.05 mol,氯化锌0.10 mol,反应温度80℃,反应时间8 h,后处理加冰水300 g为较优的反应条件,该条件下3,4,4’-三羟基二苯甲酮产率为67.2%。该合成方法工艺流程简单安全,原料易得,收率良好,有广阔的应用前景。Polyhydroxybenzophenones are a class of compounds widely used in ultraviolet absorbers.3,4,4’-trihydroxybenzophenone is synthesized in one step using phenol,3,4-dihydroxybenzoic acid as raw material,methanesulfonic acid as solvent and zinc chloride as catalyst.The effects of reaction time,reaction temperature,amount of methane sulfonic acid,amount of zinc chloride and amount of ice water after treatment on the reaction are investigated.The experimental results show that the optimal reaction conditions are 0.1 mol of 3,4-dihydroxybenzoic acid,0.1 mol of phenol,1.05 mol of methanesulfonic acid,0.10 mol of zinc chloride,reaction temperature 80℃,reaction time 8 hours,and 300 g of ice water after treatment,the yield of 3,4,4’-trihydroxybenzophenone is 67.2%under this conditions.The synthesis method is simple and safe,the raw materials are easy to obtain,the yield is good,and there are broad application prospects.

关 键 词：多羟基二苯甲酮 3 4 4’-三羟基二苯甲酮 甲烷磺酸 氯化锌 FRIEDEL-CRAFTS酰基化反应 

分 类 号：O621.3[理学—有机化学]