文档介绍:第 41 卷第 4 期
2010 年 8 月
中南大学学报(自然科学版)
Journal of Central South University (Science and Technology)
Al2O3 负载催化空气氧化 3-氧代-α-紫罗兰酮
合成 1-羟基-4-氧代-α-紫罗兰酮
唐瑞仁,李菲,张瑞荣,周亚平
(中南大学化学化工学院,湖南长沙,410083)
Aug. 2010
摘
要:以空气为氧化剂,在温和的条件下,研究三氧化铝负载下催化氧化 3-氧代-α-紫罗兰酮合成 1-羟基-4-氧
代-α-紫罗兰酮的反应,考察制备过程中反应温度、反应时间、空气湿度、 Al2O3 用量和 Al2O3 酸碱性等对反应的
影响。反应产物用 CHCl3-CH3OH 混合溶剂进行洗涤与催化剂分离,目标产物结构经 GC-MS 和 1HNMR 等测试技
术进行表征。研究结果表明:在此催化体系中,室温条件下,以粒度为 ~ µm 的中性或碱性 Al2O3 为载体,
氧化铝和反应底物的质量比为 10׃1,通入未经干燥的空气充分反应 20 h 后,3-氧代-α-紫罗兰酮转化率可到 100%,
目标化合物 1-羟基-4-氧代-α-紫罗兰酮收率达 85%;催化剂循环使用重复性良好。
关键词:氧化铝;负载;催化氧化;3-氧代α-紫罗兰酮
中图分类号:
文献标志码:A
文章编号:1672−7207(2010)04−1281−06
Catalytic synthesis of 1-hydroxy-4-oxo-α-ionone from
3-oxo-α-ionone with air supported by alumina
TANG Rui-ren, LI Fei, ZHANG Rui-rong, ZHOU Ya-ping
(School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China)
Abstract: 1-Hydroxy-4-oxo-α-ionone was synthesized from 3-oxo-α-ionone supported by alumina and air was used as
oxidant in mild conditions. Various factors were investigated, including the reaction temperature and time, air humidity,
alumina amount, acidity and basicity. The structure of product was characterized by GC-MS and 1HNMR. The results
show that at room temperature, pumping undried air to the reaction system for 20 h using neutral or alkaline alumina in
− µ