甲烷磺酸/氯化锌体系一步合成2,4,4'-三羟基二苯甲酮  

Synthesis of 2,4,4’-Trihydroxybenzophenone in One Step by Methanesulfonic Acid/Zinc Chloride System

作　　者：张琳 王子坤[1] 危云云 邓穗敏 邓方坤 Zhang Lin;Wang Zikun;Wei Yunyun;Deng Suimin;Deng Fangkun(Institute of Applied Chemistry,Jiangxi Academy of Sciences,Jiangxi,330000;Department of Environmental and Chemical Engineering,Nanchang Hangkong University,Jiangxi,330000)

机构地区：[1]江西省科学院应用化学研究所,江西330000 [2]南昌航空大学环境与化学工程学院,江西330000

出　　处：《当代化工研究》2024年第18期159-161,共3页Modern Chemical Research

基　　金：江西省科学院省级财政科研项目“柑橘黄龙病与柑橘溃疡病的防治研究”(项目编号:2022YSBG21022)。

摘　　要：多羟基二苯甲酮类化合物广泛用作紫外线吸收剂。以间苯二酚、4-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2,4,4'-三羟基二苯甲酮。试验结果表明,先4-羟基苯甲酸0.065 mol、苯酚0.05 mol、甲烷磺酸0.75 mol、氯化锌0.07 mol,反应温度80℃,反应时间4 h,后处理加冰水800 g,再用500 g水洗圆底烧瓶,合并沉淀抽滤洗涤为优选的反应条件。2,4,4'-三羟基二苯甲酮产率为98%。产物通过^(1)H、^(13)CNMR和HPLC-ESI-MS进行了表征。Polyhydroxybenzophenones are widely used in ultraviolet absorbers.2,4,4'-trihydroxybenzophenone was synthesized in one step using resorcinol,4-hydroxybenzoic acid as raw material,methanesulfonic acid as solvent and zinc chloride as catalyst.The experimental results showed that the optimal reaction conditions were 0.065 mol of 4-hydroxybenzoic acid,0.05 mol of resorcinol,0.75 mol of methanesulfonic acid,0.07 mol of zinc chloride,reaction temperature 80℃,reaction time 4 hours,and 800 g of ice water used after treatment,then 500 g water used latter for washing round bottom flash,precipitate combined,filtrated and washed.The yield of 2,4,4'-trihydroxybenzophenone was 98%.The product was characterized by ^(1)H,^(13)C NMR and HPLC-ESI-MS.

关 键 词：多羟基二苯甲酮 2 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]