超声辅助铁盐催化空气氧化制备苯偶酰  

Preparation of Benzil by Air Oxidation Catalyzed with Ferric Salts Assisted by Ultrasound

作　　者：张凯龙[1] 邵耀翔 高俊 凌宇霏 周婷婷[1] ZHANG Kai-long;SHAO Yao-xiang;GAO Jun;LING Yu-fei;ZHOU Ting-ting(College of Biological and Environmental Sciences,Zhejiang Wanli University,Zhejiang Ningbo 315100,China)

机构地区：[1]浙江万里学院生物与环境学院,浙江宁波315100

出　　处：《广州化工》2022年第21期81-84,114,共5页GuangZhou Chemical Industry

基　　金：浙江省高校实验室工作研究项目(YB202057);浙江省教育厅“十三五”省级重点建设实验教学示范中心建设项目(浙教办函[2019]218号)。

摘　　要：苯偶酰是重要的有机合成原料和药物中间体。采用超声辅助铁(Ⅲ)盐催化空气高效氧化安息香制备苯偶酰,筛选溶剂和催化剂,考察催化剂用量、氢离子浓度、温度和时间对制备的影响,柱层析纯化产品进行了多手段表征确认,并推测了可能铁盐催化空气氧化机理。结果表明DMSO为最佳溶剂,FeNO_(3)·9H_(2)O为最佳催化剂,当安息香投加量为2.1 g,超声功率180 W,催化剂投加量0.2 g,氢离子浓度1.2 mol/L,反应温度80℃,反应60 min产率达到96.1%。实验结果为高效氧化制备苯偶酰类化合物提供了新思路和方法。Benzil is an important organic synthesis material and pharmaceutical intermediate.A high efficient ferric catalytic oxidation method of benzoin was developed with air by assisted of ultrasound.The effects of various factors on synthesis were investigated,including solvent,species and quantity of catalyst,acidity,temperature and times,Furthmore,the product purified by column chromatography was characterized and confirmed by multiple analysis approaches,and the possible mechanism of ferric salt catalyzed air oxidation was speculated.The results showed that DMSO and ferric nitrate was the best solvent and catalyst,the optimal condition was with 2.1 g benzoin,180 W ultrasound power,0.2 g catalyst,hydrogen ion concentration 1.2 mol/L,at temperature of 80℃,reaction time of 60 min and yield up to 96.1%.It provided a new idea and method for preparation of benzils with high efficient and green oxidants.

关 键 词：安息香 苯偶酰 铁离子 空气 催化氧化 

分 类 号：O625[理学—有机化学]