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。
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.
出处
《化学工业与工程》
CAS
2013年第3期24-27,共4页
Chemical Industry and Engineering
