Tetra-n-butylammonium hexafluorophosphate

Tetra-n-butylammonium hexafluorophosphate [3109-63-5] M 387.5, m 239-241 . Recrystd from satd EtOH/water and dried for lOh in vac at 70°. It was also recrystd three times from abs EtOH and dried for 2 days in a drying pistol under vac at boiling toluene temperature [Bedard and Dahl J Am Chem Soc 108 5933 1986],... 

The triple degeneracy of the LUMO of Cgo was confirmed experimentally in several steps between 1990 and 1992 with the detection of Cgo and Cgo [27], Cgo - [28], Cgo - [29], Cgo - [30], and finally Cgo [31]. Owing to limitations in the solvent potential window, the elusive hexaanion species was only detected when the experiment was carried out under vacuum, at low temperature (—lO C), and using a 0.1 M tetra-n-butylammonium hexafluorophosphate (TBAPFg) electrolyte solution in a solvent mixture consisting of toluene/acetonitrile (PhMe/MeCN) in a 4 to 1 ratio. Under these conditions, using cyclic voltammetry (CV)... 

Tetra-n-butylammonium hexafluorophosphate.m 100 g (270 mmol) of (n-Bu)4NI is dissolved in a minimum quantity of acetone. To this is added, with stirring, an acetone solution that contains 50 g (310 mmol) of (NH4)PF6. It is important to maintain at least a 5 % excess of PFg. The resultant mixture is filtered to remove the precipitate of NH4I. Then water is added to precipitate (n-Bu)4NPF6, which is collected by filtration and washed several times with water to remove all ammonium salts. The crude product is again precipitated... 

Chemicals and Solvents. Acetonitrile (Burdick and Jackson) and dichloromethane (Fisher) were stored over Davisson 3 molecular sieves for at least 24 h. before use. Tetra-n-ethylammonium hexafluorophosphate (TEAH) was purchased from Alfa and used without further purification. Tetra-n-ethylammonium perchlorate (TEAP) was prepared from the corresponding bromide salt (Eastman) with the use of a previously published procedure (7). Tetra-n-butylammonium hexafluorophosphate (TBAH) was prepared by dissolving the iodide salt (Eastman) in a hot, equivolume water/ethanol/ acetone mixture followed by addition of HPFg (Alfa). The solution was reduced to approximately half its original volume, then cooled to room temperature. The resulting white solid was filtered off... 

In dichloromethane at 25 °C 0.1 M tetra-n-butylammonium hexafluorophosphate supporting electrolyte potentials referenced to ferrocene. 

Synthesis. Diphenyliodonium hexafluorophosphate, Ph2lPF6, and triphenylsulfonium hexafluoroantimonate, PhaSSbFe, were synthesized using literature procedures (25). Tetra-n-butylammonium hexafluorophosphate, TBAPFe, was obtained by direct metathesis between tetra-n-butylammonium bromide (99%) and potassium hexafluorophosphate (tech.), KPFe. 

Tetra-n-butylammonium hexafluorophosphate. Saturated sodium chloride calomel electrode. 

Acid" NMF samples gave pH readings of 6-8 "alkaline" NMF samples gave pH = 10-11. The supporting electrolyte for electrochemical experiments was tetra-n-butylammonium hexafluorophosphate (TBAPFe) from Southwestern Analytical Chemicals. 

Since contact ion pairs can be separated by the deliberate addition of an inert salt (such as tetra-n-butylammonium perchlorate or hexafluorophosphate) [132], (Eq. 11) ... 

Tebbe olefination, 441 Tebbe olefinations, 368 Tebbe s reagent, 457 Tedania ignis, 246 Tedanolide, 246 tedanolide, 256 TEMPO, 250, 301 temporary silicon tether, 103 Tennant quinoline synthesis, 7 tetra-n-butylammonium fluoride (TBAF), 214 2-(7-aza-1 H-benzotriazole-1 -yl)-1,1,3, 3-tetramethyluronium hexafluorophosphate (HATU), 25... 

The addition of small amounts of inert salts such as tetra-n-butylammonium perchlorate or hexafluorophosphate induces large decreases in the intensity of the charge-transfer absorption bands owing to the facile exchange of the intimate charge-transfer ion pair e.g. 

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