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作 者:冯里[1] 王晓丽[1] 褚朝森[1,2] 彭飞宏 徐文 冷志新
机构地区:[1]江苏联合职业技术学院连云港中医药分院,江苏连云港222007 [2]连云港市药物研发共性技术中心,江苏连云港222007
出 处:《当代化工》2017年第9期1768-1770,共3页Contemporary Chemical Industry
基 金:江苏省青蓝工程培养基金(2014-2017)
摘 要:以苯乙腈,1,2-二溴乙烷为原料,四丁基溴化铵为相转移催化剂,氢氧化钾为碱性试剂,在超声波作用下实现了苯乙腈的环丙烷化反应。以苯乙腈12 mmol为模型,考查了超声频率、溶剂种类、溶剂用量、氢氧化钾用量、时间对反应的影响。研究结果表明,最佳反应条件为40 k Hz下、甲苯做溶剂、溶剂用量20 m L、氢氧化钾与苯乙腈摩尔比为10∶1、反应4 h。反应转化率达97.9%,选择性为96.2%,收率达94.2%。Using benzeneacetonitrile and 1, 2-dibromoethane as starting materials, TBAB as phase transfer catalyst, KOH as alkaline reagent, cyclopropanation of benzeneacetonitrile was implemented under ultrasonic condition. Taking 12 mmol benzeneacetonitrile as research object, effect of ultrasonic frequency, solvent type, solvent dosage, KOH dosage and reaction time on the cyclopropanation was studied. The result showed that the optimum reaction condition was as follows: 40 k Hz, using 20 m L toluene as solvent, mole ratio of KOH and benzeneacetonitrile 10:1, reaction time 4 h. Under above conditond,the yield reached to 94.2%, the conversion rate was 97.9% convertion and the selectivity was 96.2%.
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