| 2-甲基-4-甲醛肟基苯甲酸甲酯的合成 |
| |
| 引用本文： | 黄道友,江国栋,王勇,李立威,袁颂东.2-甲基-4-甲醛肟基苯甲酸甲酯的合成[J].化学试剂,2017,39(7). |
| |
| 作者姓名： | 黄道友 江国栋 王勇 李立威 袁颂东 |
| |
| 作者单位： | 1. 湖北工业大学化学化工学院,湖北武汉,430068;2. 荆楚理工学院湖北省荆门医药工业技术研究院,湖北荆门,448000 |
| |
| 基金项目： | 湖北省教育厅科学技术中青年人才项目，湖北省自然科学基金创新群体重点项目，荆楚理工学院博士人才科研启动基金资助项目，荆楚理工学院药物合成与优化湖北省重点实验室开放基金资助项目 |
| |
| 摘 要： | 以2-甲基-4-溴苯甲酸为起始原料,经酰化和酯化反应制得2-甲基-4-溴苯甲酸甲酯,2-甲基-4-溴苯甲酸甲酯与氰化亚铜在DMF中发生取代反应得到2-甲基-4-氰基苯甲酸甲酯,接着与盐酸羟胺在碳酸钠存在下反应得到标题化合物,总收率为61%,纯度为99.2%。化合物的结构经IR、MS、~1HNMR和~(13)CNMR等确证。该路线中目标产物肟经由氰基直接一步反应制得,工艺简单可靠、产品收率高。该方法为肟的合成提供了良好的实验基础。
|
| 关 键 词： | 2-甲基-4-溴苯甲酸 肟 合成 |
Synthesis of 4-(Hydroxyimino-methyl)-2-methyl Benzoic Acid Methyl Ester |
| |
| HUANG Dao-you,JIANG Guo-dong,WANG Yong,LI Li-wei,YUAN Song-dong.Synthesis of 4-(Hydroxyimino-methyl)-2-methyl Benzoic Acid Methyl Ester[J].Chemical Reagents,2017,39(7). |
| |
| Authors: | HUANG Dao-you JIANG Guo-dong WANG Yong LI Li-wei YUAN Song-dong |
| |
| Abstract: | In this work,4-bromo-2-methyl benzoic acid methyl ester was synthesized by acylated and esterified,with 2-methyl-4-bromo-benzoic acid as starting material.4-Cyano-2-methyl-benzoic acid methyl ester was obtained by reaction of 4-bromo-2-methyl benzoic acid methyl ester with CuCN in DMF solution.Reaction of 4-cyano-2-methyl-benzoic acid methyl ester with hydroxylamine hydrochloride in the presence of Na2CO3 affords product 4-(hydroxyimino-methyl)-2-methyl benzoic acid methyl ester.The total yield is 61％ and its purity is 99.2％.All the compounds were fully characterized by IR,MS,1HNMR and 13CNMR,and all these datas indicate that compounds have been successfully prepared.This route from cyano to oxime is only one step,and this method is in simple operation and high yield.The method also provides a good experimental foundation for the synthesis of oxime. |
| |
| Keywords: | 4-bromo-2-methyl benzoic acid methyl ester oxime synthesis |
| 本文献已被 CNKI 万方数据 等数据库收录！ |
|
