| 5-氨基-1,4-苯并二恶烷盐酸盐的合成 |
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| 引用本文： | 初晓辉,陈锦春. 5-氨基-1,4-苯并二恶烷盐酸盐的合成[J]. 广州化工, 2014, 0(11): 68-70 |
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| 作者姓名： | 初晓辉 陈锦春 |
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| 作者单位： | 烟台大学化学化工学院,山东烟台264005 |
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| 基金项目： | 烟台大学博士科研启动基金项目（HY07B30）. |
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| 摘 要： | 以2,3-二羟基苯甲酸为原料,经酚羟基烷基化保护、羧酸叠氮化、Curtius重排、水解成盐四步反应以35%的总收率合成了5-氨基-1,4-苯并二恶烷盐酸盐,其结构经1H-NMR确认。由于合理的反应溶剂选择和反应温度控制,减少了副反应的发生、简化了工艺操作、降低了分离难度、提高了收率和产品纯度,使得该路线适合于工业化生产。
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| 关 键 词： | -二羟基苯甲酸 Curtius重排 -氨基- -苯并二恶烷 合成 |
Synthesis of 2,3-dihydrobenzo[ b] [1,4] dioxin-5-amine |
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| CHU Xiao-hui,CHEN Jin-chun. Synthesis of 2,3-dihydrobenzo[ b] [1,4] dioxin-5-amine[J]. GuangZhou Chemical Industry and Technology, 2014, 0(11): 68-70 |
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| Authors: | CHU Xiao-hui CHEN Jin-chun |
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| Affiliation: | ( School of Chemistry and Chemical Engenerring, Yantai University, Shandong Yantai 264005, China) |
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| Abstract: | By using 2,3-dihydroxybenzoic acid as initial material, 2,3-dihydrobenzo[b][1,4]dioxin-5-amine hydrochloride was synthesized via alkylation of phenolic hydroxyl group , azidation of carboxylic acid , Curtius rearrangement , hydrolysis and salification with a overall yield of 35%.Structure of product was characterized by 1 H-NMR analysis.Benefit from proper choice of solvent and reaction temperate.This route encompassed fewer side reations , simplified synthetic and isolation process , and increased yield with higher purity , which was suitable for large -scale preparation. |
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| Keywords: | 2,3 -Dihydroxybenzoic acid Curtius rearrangement 2,3 -Dihydrobenzo [ b] -[1,4] dioxin -5 -amine synthesis |
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