| 第 36 卷第 4 期 |  | Vol. 36 No. 4 | | 2006 年 8 月 | Aug 2006 |
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所屬欄目：醫藥及中間體
5-溴香蘭素的合成 |
| 劉穎; 宋志軒; 楊煥新; 張龍(長(cháng)春工業(yè)大學(xué)化學(xué)工程學(xué)院; 吉林工業(yè)職業(yè)技術(shù)學(xué)院; 吉林長(cháng)春; 吉林吉林) |
| 摘 要：以甲基香蘭素為原料,氫溴酸與過(guò)氧化氫為溴化劑,溴化鋁為催化劑,無(wú)水乙醇為溶劑制備5-溴香蘭素。實(shí)驗確定了制備過(guò)程的適宜工藝條件:將甲基香蘭素(0.07mol)用無(wú)水乙醇使其完全溶解,攪拌下按摩爾比n(C8H8O3)∶n(HBr)∶n(H2O2)=0.07∶0.59∶0.10加入40%的氫溴酸和30%的過(guò)氧化氫,加入少量溴化鋁(催化劑),控制反應溫度不超過(guò)5～10℃,反應時(shí)間6h。在此條件下產(chǎn)物收率為98.3%,優(yōu)于現有的合成工藝。 |
| 關(guān)鍵詞：5-溴香蘭素; 溴化反應; 3; 4; 5-三甲氧基苯甲醛 |
| 中圖分類(lèi)號：TQ244.1 文獻標識碼：A 文章編號：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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