2,3,4-三羟基二苯酮的新合成工艺

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。

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	刘兰香
	伊冠东
	张雯雯
	李坤
	冀浩博
	陈赤清
	刘义稳
	张弘

关键词： 2,3,4-三羟基二苯酮；合成；工艺

Abstract： The important industrial material 2,3,4-trihydroxydiphenyl (3HBP) 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 3HBP 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 3HBP was 89.1% tested by column chromatography. The method was simple, environmentally friendly and had value potential of industrial application.

Keywords： 2, 3, 4-trihydroxydiphenyl； synthesis； optimum process

Received 2019-01-10;

Fund:国家重点研发计划资助（2018YFD0600404）。

Corresponding Authors: 张弘,E-mail:kmzhhong@163.com。 Email: kmzhhong@163.com

About author: 刘兰香(1986-),女,助理研究员,现从事天然产物资源化学方面的研究。

引用本文:

刘兰香, 伊冠东, 张雯雯, 李坤, 冀浩博, 陈赤清, 刘义稳, 张弘.2,3,4-三羟基二苯酮的新合成工艺[J]. 化学工业与工程, 2019,36(6): 17-22

Liu Lanxiang, Yi Guandong, Zhang Wenwen, Li Kun, Ji Haobo, Chen Chiqing, Liu Yiwen, Zhang Hong.A New Method for the Synthesis of 2, 3, 4-Trihydroxybenzophenone[J]. Chemcial Industry and Engineering, 2019,36(6): 17-22

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