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作 者:宁志强[1] 徐虹[1] 杨杰[1] 刘宁生[1] 于明慧[1] 李猛[1]
机构地区:[1]黑龙江省科学院石油化学研究院,黑龙江哈尔滨150040
出 处:《化学与粘合》2013年第1期50-52,70,共4页Chemistry and Adhesion
摘 要:2-萘硼酸是有机硼酸中一个重要的中间体。以2-溴萘为原料,使用格氏试剂法合成2-萘硼酸。考察了中试规模物料配比,格氏试剂反应条件及亲核反应的反应条件,优化并确定了反应条件。优化的反应条件如下,2-溴萘∶镁屑∶硼酸三甲酯=1∶1.05∶1.5,格氏试剂反应温度60℃,硼酸反应温度为(-25±2)℃,格氏试剂反应时间3h,硼酸反应时间为3h,产品收率72.4%。该反应避免了昂贵易燃的丁基锂,使生产成本大为降低。The 2-naphthaleneboronic acid is an important immediate in organic boric acid. It was prepared by Grignard reagent method from 2- bromo naphthalene. The reaction conditions, including materials ratios, Grignard reagent and nucleophilic reaction conditions were investigated in pilot scale. The optimized reaction conditions were confirmed. The optimal reaction conditions were listed as follows: the ratio of 2-bromonaphthalene to Mg to trimethylborate=1:1.05:1.5, reaction temperature in Grignard reaction and boric acid was 60℃ and (-25±2)℃ respectively, reaction time both in Grignard reaction and boric acid was 3h. Under these conditions, the yield was 72.4%. This method avoided using expensive BuLi, the production costs were reduced greatly.
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