第 38 卷第 3 期Vol. 38 No. 3
2008 年 6 月Jun 2008

所属栏目:农药及中间体

邻甲代烯丙氧基苯酚合成呋喃酚工艺研究
孔祥云1,蒋 彪1,2,罗和安1 (1. 湘潭大学 化工学院,湖南 湘潭 411105;2. 湖南化工研究院 国家农药创制工程技术研究中心,湖南 长沙 410007)
摘 要:以邻甲代烯丙氧基苯酚为原料,异丙醇铝为催化剂,在溶剂二甲苯的条件下,经过Claisen重排和环合反应合成呋喃酚。重点研究了物料配比、反应溶剂、反应温度、反应时间对反应的影响,优化条件为:邻甲代烯丙氧基苯酚浓度为32%(m / m),异丙醇铝3.0%(m / m),反应温度高于150℃,反应时间10 h。此条件下反应的转化率可以达到96%以上,选择性78%,收率75%。
关键词:邻甲代烯丙氧基苯酚;呋喃酚;环合反应;工艺研究
中图分类号:TQ251.1  文献标识码:A  文章编号:1009-9212(2008)03- 0015-03
Synthesis of Benzofuranol from Methallyloxyphenol
KONG Xiang-yun1,JIANG Biao1,2,LUO He-an1 (1. School of Chemical Engineering,Xiangtan University,Xiangtan 411105,China;2. National Engineering Research Centre for Agrochemicals,Hunan Research Institute of Chemical Industry,Changsha 410007,China)
Abstract:In the preparation of benzofuranol from methallyloxyphenol through Claisen- rearrangement and cyclization, aluminium isopropoxide was used as catalyst,xylene was used as solvent. The material ratio,solvent,reaction temperature and reaction time were studied. The optimum reaction conditions were determined as follows:n(methallyl- oxyphenol) ∶ n(xylene)=1 ∶ 3,the mass fraction of aluminium isopropoxide is 3.0%,the temperature was higher than 150℃,the reaction time was 10 h. Under these operation conditions,the conversion was over 96%,selectivity was 78%,the yield of benzofuranol was 75%.
Key words:methallyloxyphenol ;benzofuranol;cyclization;optimization
基金项目:湖南省自然科学基金资助项目(05JJ30025)。
作者简介:孔祥云(1981-),男,湖南长沙人,硕士研究生,主要从事化学工程与工艺研究。
联 系 人:罗和安,教授。(E-mail:hluo@xtu.edu.cn)
收稿日期: 2008-06-0