Safe preparation and purification of sodium tetrakis[(3,5-trifluoromethyl)phenyllborate (NaBArF24):: Reliable and sensitive analysis of water in solutions of fluorinated tetraarylborates
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Yakelis, NA
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机构:Univ Calif Berkeley, Lawrence Berkeley Lab, Div Chem Sci, Berkeley, CA 94720 USA
Yakelis, NA
Bergman, RG
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Univ Calif Berkeley, Lawrence Berkeley Lab, Div Chem Sci, Berkeley, CA 94720 USAUniv Calif Berkeley, Lawrence Berkeley Lab, Div Chem Sci, Berkeley, CA 94720 USA
Bergman, RG
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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
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)).