Safe preparation and purification of sodium tetrakis[(3,5-trifluoromethyl)phenyllborate (NaBArF24):: Reliable and sensitive analysis of water in solutions of fluorinated tetraarylborates

被引:287
作者
Yakelis, NA
Bergman, RG [1 ]
机构
[1] Univ Calif Berkeley, Lawrence Berkeley Lab, Div Chem Sci, Berkeley, CA 94720 USA
[2] Univ Calif Berkeley, Dept Chem, Berkeley, CA 94720 USA
关键词
D O I
10.1021/om0501428
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
A safe, convenient preparation of the reagent sodium tetrakis[(3,5-trifluoromethyl)phenyl]borate (NaBArF24) has been devised by utilizing a magnesium-bromine exchange reaction in the absence of metallic magnesium. Purified material was then rigorously dried over P2O5 (NaBArF24 with < 500 ppm H2O by mass) or recrystallized as a hydrate (NaBArF24 center dot(2.6 +/- 0.1)H2O). Accurate analysis of the water content of these samples by H-1 NMR was accomplished by using dimethylzirconocene (Cp2Zr(CH3)(2)).
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页码:3579 / 3581
页数:3
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