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3-羟基-4-甲氧基苯甲醛的合成与表征
引用本文:殷建平,王芳斌,黄可龙,于金刚.3-羟基-4-甲氧基苯甲醛的合成与表征[J].精细化工,2006,23(5):460-462,520.
作者姓名:殷建平  王芳斌  黄可龙  于金刚
作者单位:中南大学,化学化工学院,湖南,长沙,410083
摘    要:以对羟基苯甲醛为原料,经溴代、甲基化和水解3步反应合成了异香兰素,改进并优化了合成路线。溴代采用三氯甲烷作为溶剂,在0℃的条件下反应6 h,n(对羟基苯甲醛)∶n(溴素)=1∶1.05;确定了水解反应的最佳条件:氯化亚铜作催化剂,于130℃反应4 h。反应总收率达62%以上。用IR,1HNMR确证了中间体和产物的结构。

关 键 词:异香兰素  溴代  甲基化  水解
文章编号:1003-5214(2006)05-0460-04
收稿时间:2005-10-27
修稿时间:2005-10-272005-12-28

Synthesis and Characterization of 3-Hydroxy- 4-methoxybenzaldehyde
YIN Jian-ping,WANG Fang-bin,HUANG Ke-long,YU Jin-gang.Synthesis and Characterization of 3-Hydroxy- 4-methoxybenzaldehyde[J].Fine Chemicals,2006,23(5):460-462,520.
Authors:YIN Jian-ping  WANG Fang-bin  HUANG Ke-long  YU Jin-gang
Abstract:Starting from p-hydroxybenzaldehyde,isovanillin(3-hydroxy-4-methoxybenzaldehyde) was synthesized by three-step reactions of bromination,methylation and hydrolysis.Bromination was run at 0 ℃ for 6 h with chloroform as solvent and molar ratio of p-hydroxybenaldehyde bromine 1∶1.05.Hydrolysis was carried out with cuprous chloride as catalyst at 130 ℃ for 4 h.The overall yield of the reactions was over 62%.Structures of the product and intermediate compounds were characterized by IR and ~1HNMR.
Keywords:isovanillin  bromination  methylation  hydrolysis
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