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。
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.
出处
《广州化工》
CAS
2014年第11期68-70,共3页
GuangZhou Chemical Industry
基金
烟台大学博士科研启动基金项目(HY07B30)
