四[（3,5-三氟甲基）苯基]硼酸钠（NaBArF(24)）：水合作用的安全制备、标准化纯化及分析
Sodium Tetrakis[(3,5-trifluoromethyl)phenyl]borate (NaBArF(24)): Safe Preparation, Standardized Purification, and Analysis of Hydration.
作者信息
Yakelis Neal A, Bergman Robert G
机构信息
Department of Chemistry, University of California, Berkeley, California 94720.
出版信息
Organometallics. 2005 Jul 4;24(14):3579-3581. doi: 10.1021/om0501428.
Abstract
A safe, convenient preparation of the reagent sodium tetrakis[(3,5-trifluoromethyl)phenyl]borate (NaBArF(24)) has been devised by utilizing a magnesium-bromine exchange reaction in the absence of metallic magnesium. Purified material was then rigorously dried over P(2)O(5) (NaBArF(24) with < 500 ppm H(2)O by mass) or recrystallized as a hydrate (NaBArF(24).2.6 +/- 0.1H(2)O). Accurate analysis of the water content of these samples by (1)H NMR was accomplished by using dimethylzirconocene [Cp(2)Zr(CH(3))(2)].
摘要
通过在无金属镁的情况下利用镁-溴交换反应，设计出了一种安全、便捷的制备试剂四[（3,5-三氟甲基）苯基]硼酸钠（NaBArF(24)）的方法。然后将纯化后的物质在P(2)O(5)上严格干燥（质量分数<500 ppm H(2)O的NaBArF(24)），或重结晶为水合物（NaBArF(24).2.6±0.1H(2)O）。通过使用二甲基锆茂[Cp(2)Zr(CH(3))(2)]，利用(1)H NMR对这些样品的水分含量进行了准确分析。
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