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化学工业与工程 2013, Vol. 30 Issue (3) :24-27    DOI:
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二乙基(3-吡啶基)硼烷的合成
 张静1, 靳凤民2
1.天津大学仁爱学院;2.天津大学化工学院
Synthesis of Diethyl (3-Pyridyl) borane
 ZHANG  Jing1, JIN  Feng-Min2
1.Renai College of Tianjin University;2. School of Chemical Engineering and Technology, Tianjin University

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摘要 以3-溴吡啶和二乙基甲氧基硼烷为原料合成了二乙基(3-吡啶基)硼烷。探索了反应时间、反应温度、反应配比等反应条件对于反应收率的影响。结果表明最适宜合成工艺条件为:反应温度0~5 ℃,反应时间6 h,二乙基甲氧基硼烷滴加时间30 min,物料配比n(3-溴吡啶)∶n(二乙基甲氧基硼烷)为0.9∶1.0,物料配比n(异丙基氯化镁)∶n(二乙基甲氧基硼烷)为1.0∶1.0。在最适宜工艺条件下制得产品为白色固体,熔点为172~175 ℃,产率在81%以上。并通过质谱和红外光谱对其进行了结构表征。
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张静
靳凤民
关键词有机硼烷   二乙基(3-吡啶基)硼烷   异丙基氯化镁     
Abstract: Diethyl (3-pyridyl) borane was prepared from 3-bromopyridine and diethylmethoxyborane. The effects of reaction time,temperature and molar ratio of the material on the reaction were studied. The experimental result showed that the optimum condition were: reaction time was 6 h, reaction temperature was 0—5 ℃, dropping time of diethylmethoxyborane was 30 min, molar ratio of 3-bromopyridine to diethylmethoxyborane was 0.9∶1.0, and molar ratio of diethylmethoxyborane to isopropyl magnesium chloride was 1.0∶1.0. The product was white solid with melting point of 172—175 ℃, the yield of product was up to 81%. IR and MS were used to characterize the structure of product.
Keywordsorganic borane   diethylmethoxyborane   isopropyl magnesium chloride     
Received 2012-10-26;
Corresponding Authors: 靳凤民,电话:(022)87401887,E-mail: fmjin@tju.edu.cn。     Email: fmjin@tju.edu.cn
About author: 张静(1979-),女,高级工程师,主要研究方向:药物及中间体合成;精细化学品合成。
引用本文:   
张静, 靳凤民.二乙基(3-吡啶基)硼烷的合成[J].  化学工业与工程, 2013,30(3): 24-27
ZHANG Jing, JIN Feng-Min.Synthesis of Diethyl (3-Pyridyl) borane[J].  Chemcial Industry and Engineering, 2013,30(3): 24-27
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