| 第 36 卷第 4 期 |  | Vol. 36 No. 4 | | 2006 年 8 月 | Aug 2006 |
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所属栏目：医药及中间体
5-溴香兰素的合成 |
| 刘颖; 宋志轩; 杨焕新; 张龙(长春工业大学化学工程学院; 吉林工业职业技术学院; 吉林长春; 吉林吉林) |
| 摘 要：以甲基香兰素为原料,氢溴酸与过氧化氢为溴化剂,溴化铝为催化剂,无水乙醇为溶剂制备5-溴香兰素。实验确定了制备过程的适宜工艺条件:将甲基香兰素(0.07mol)用无水乙醇使其完全溶解,搅拌下按摩尔比n(C8H8O3)∶n(HBr)∶n(H2O2)=0.07∶0.59∶0.10加入40%的氢溴酸和30%的过氧化氢,加入少量溴化铝(催化剂),控制反应温度不超过5～10℃,反应时间6h。在此条件下产物收率为98.3%,优于现有的合成工艺。 |
| 关键词：5-溴香兰素; 溴化反应; 3; 4; 5-三甲氧基苯甲醛 |
| 中图分类号：TQ244.1 文献标识码：A 文章编号：1009-9212(2006)04-0024-02 |
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| Preparation of 5-Bromo-vanillin Aldehyde |
| LIU Ying1; SONG Zhi-xuan2; YANG Huan-xin1; ZHANG Long1 （1. School of Chemical Engineering; Changchun University of Technology; Changchun 130012; China; 2. Institute of Jilin Occupational Training; Jilin 130020; China） |
| Abstract：A new process for the preparation of 5-bromo-vanillin with vanillic aldehyde as raw material,AlBr3 as activator,HBr and H2O2 as brominating agent and anhydrous alcohol as solvent was developed in this paper. Through an investigation on effect of reaction parameters on the yield of 5-bromo-vanillin,suitable reaction conditions were obtained as following: vanillin aldehyde(0.07 mol)was dissolved completely in anhydrous alcohol,and 40% HBr and 30% H2O2 added in solution based on the rate n(C8H8O3) : n(HBr) : n... |
| Key words：5-bromo-vanillin; bromination; 3; 4; 5-trimethoxybenzal dehyde |
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收稿日期：2005-09-22
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