文献类型：期刊文献

中文题名：2,3,4-三羟基二苯酮的新合成工艺

英文题名：A New Method for the Synthesis of 2, 3, 4-Trihydroxybenzophenone

作者：刘兰香[1] 伊冠东[1] 张雯雯[1] 李坤[1] 冀浩博[1] 陈赤清[2] 刘义稳[2] 张弘[1]

第一作者：刘兰香

机构：[1]中国林业科学研究院资源昆虫研究所,国家林业和草原局特色森林资源工程技术研究中心,昆明650224;[2]五峰赤诚生物科技股份有限公司,国家林业和草原局五倍子高效培育与精深加工工程技术研究中心,湖北五峰443400

年份：2019

卷号：36

期号：6

起止页码：17-22

中文期刊名：化学工业与工程

外文期刊名：Chemical Industry and Engineering

收录：CSTPCD;;CSCD:【CSCD2019_2020】；

基金：国家重点研发计划资助(2018YFD0600404)

语种：中文

中文关键词：2,3,4-三羟基二苯酮;合成;工艺

外文关键词：2,3,4-trihydroxydiphenyl;synthesis;optimum process

分类号：TQ572.4;TQ460.4

摘要：以焦性没食子酸为原料,甲醇-水为混合溶剂,草酸-磷酸为催化剂,氮气保护的条件下与三氯甲苯反应,合成了重要的工业材料2,3,4-三羟基二苯酮(3HBP),反应条件温和。通过单因素实验确定了合成3HBP的最适宜工艺条件为:焦性没食子酸的质量为6.3 g(0.05 mol),混合溶剂甲醇-水(体积比为2∶8)为50.0 mL,升温至40℃时缓慢滴加三氯甲苯(0.055 mol),滴加完毕后升温至65℃恒温反应至原料焦性没食子酸消失。在最适宜条件合成的3HBP,经柱层析后收率为89.1%。该合成方法简便,环境污染小,绿色环保,具有工业化应用的潜力。
The important industrial material 2,3,4-trihydroxydiphenyl(3 HBP) was synthesized from pyrogallic acid and benzotrichloride, oxalate and phosphoric acid as the catalyst, methanol-water as mixed solvents in the nitrogen atmosphere. The results of single factor experiments show that the optimum process conditions for synthesis of 3 HBP are: Pyrobitumen gallic acid is 6.3 g(0.05 mol), the methanol-water mixed solvents(volume ratio 2∶8) is 50.0 mL, benzotrichloride(0.055 mol) is added slowly when the mixture solution is 40 ℃, and then the temperature of the mixture solution is kept at 65 ℃ until the pyrogallic acid disappear. The yield of 3 HBP was 89.1% tested by column chromatography. The method was simple, environmentally friendly and had value potential of industrial application.