格氏试剂生成条件下原位一锅法合成3,4-二烷氧基苯硼酸  

One-pot Synthesis of 3,4-Dialkoxyphenylboronic Acids in Situ under Grignard Reagent Generated Conditions

作　　者：张强[1] 史娟[1] 田光辉[1] 姜敏[1] 杨海涛[1] 

机构地区：[1]陕西理工大学化学与环境科学学院陕西省催化基础与应用重点实验室,陕西汉中723001

出　　处：《化学试剂》2016年第9期903-906,共4页Chemical Reagents

基　　金：国家自然科学基金资助项目(21502109);陕西省教育厅专项科研计划项目(15JK1161);陕西理工学院人才启动项目(SLGKYQD2-09)

摘　　要：在格氏试剂生成条件下,将3,4-二烷氧基溴苯、硼酸三异丙酯、镁粉、1,2-二溴乙烷、无水氯化锂、环戊基甲醚一锅法高效合成目标化合物,并采用~1HNMR、^(13)CNMR对其进行表征。该方法采用环戊基甲醚解决了传统制备格氏试剂方法收率不高、溶剂不易回收等缺点,具有操作简捷、能耗低、绿色环保、成本低廉等优点。该合成方法为目标化合物的应用奠定了基础,同时为其他芳基硼酸的合成与应用提供了实用的合成思路。Four kinds of 3,4-dialkoxyphenylboronic acids were efficiently synthesized via one-pot reaction employing correspond- ing aryl bromides and triisopropyl borate as the reactant, anhydrous lithium chloride and 1,2-dibromoethane as the co-additives under Grignard reagent generated conditions in eyclopentyl methyl ether. The target molecules were confirmed by ^1HNMR and ^13CNMR. This protocol overcomes the shortcoming of low yield rate of traditional Grignard reagent, adopts the cyclopentyl methyl ether as the recyelable solvent and the anhydrous lithium chloride as the additive,which constitutes the advantages of simple operation,low energy consumption, green environmental protection, low cost, etc. Moreover, these can be envisaged to serve as new launching plat forms for the application 3,4-dialkoxyphenylboronic acids and the preparation of other aryl boric acid synthesis.

关 键 词：3 4-二烷氧基苯硼酸 格氏反应 环戊基甲醚 

分 类 号：O622.2[理学—有机化学]