第 36 卷第 1 期 Vol. 36 No. 1 2006 年 2 月 Feb 2006

所属栏目：医药及中间体 HIV病毒抑制剂中间体5-戊基间苯二酚的合成

徐宇伦; 张龙; 金鑫; 宋义新(长春工业大学化工学院; 大连兆科生化有限公司; 吉林长春; 辽宁大连)

摘　要：以3,5-二甲氧基苯甲酸为起始原料,与LiH在室温下反应5h生成苯甲酸盐,生成的盐再与正丁基锂进行酰化反应得到3,5-二甲氧基苯戊酮,进而在210℃以下进行乌尔夫-黄鸣龙反应将酮还原,生成3,5-二甲氧基戊苯,所得产物与吡啶盐酸盐熔融,于200℃回流2h,脱甲基制得5-戊基间苯二酚,总收率达60.9%,纯度≥98%。

关键词：3; 5-二甲氧基苯甲酸; 酰化; 乌尔夫-黄鸣龙还原; 5-戊基间苯二酚

中图分类号：TQ243.1　　文献标识码：A　　文章编号：1009-9212(2006)01-0027-03

Synthesis of HIV Inhibitor Intermediate 5-Pentyl Resorcinol

XU Yu-lun1; ZHANG Long1; JIN Xin2; SONG Yi-xin2（1.School of Chemical and Engineering; Changchun University of Technology; Changchun 130012; China; 2.Dalian Zhaoke Biochemical Co.; Ltd; Dalian 116620; China）

Abstract：3,5-Dimethoxybenzoic acid reacts with lithium hydride to form salt which is acylated by n-butyllithium to synthesize 1-(3,5-dimethoxyphenyl)-1-pentanone,and then this ketone is reduced by Wolff L-Huangminglong reaction under 210 ℃ to form 3,5-dimethoxy-1-phenylbenzene that refluxs with pyridine and concentrated hydrochloric acid for 2 h at 200 ℃ to prepare 5-pentyl resorcinol.The total yield of 5-pentyl resorcinol is up to 60.9% and its purity is no less than 98%.

Key words：3; 5-dimethoxybenzoic acid; acylation; Wolff L-Huangminglong reaction; 5-pentyl resorcinol

收稿日期：2005-09-11

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