Compound [3b]PF6

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InChIKey VBDBMZJFSDMZBZ-UHFFFAOYSA-N

Compound data: 1H NMR

Compound data: 19F NMR

Compound data: Crystallographic data

Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.

A 250 mL round-bottom flask was charged with FeCl₃·6H₂O (0.07 g, 0.26 mmol), 2b (0.200 g, 0.52 mmol), NaPF₆ (0.043 g, 0.26 mmol), and NaO^tBu (0.050 g, 0.52 mmol). MeOH (50 mL) was added and the flask was stirred and refluxed at 100 °C overnight. The flask was then cooled to room temperature and the solvent removed. The brown solid was dissolved in minimal CH₂Cl₂ and added slowly to 100 mL of pentane to precipitate the compound. The mixture was then filtered and the solid collected. Isolated yield = 0.180 g (72 %). ¹H NMR (CDCl₃, 300 MHz, 25 °C): δ 29.0 (br), 19.3 (br), 11.1 (s), 10.6 (s), 3.1 (s), 2.9 (s), -8.9 (br), -29.6 (br), -31.9 (br), -49.9 (br), -56.5 (br), -61.4 (v br), -64.7 ppm (v br). ¹⁹F NMR (CDCl₃, 282 MHz, 25 °C): δ -70.6 (d, 6F, J = 712.8 Hz, PF₆), -82.0 ppm (s, 3F, CF₃). UV-Vis (CH₃CN): λ (ε) 312 (sh), 412 (22 630), 505 (11 100), 996 nm (4 000 M^-1 cm^-1). μ_eff (Evans method) = 1.72 μ_B. Anal. Calcd for FeC₄₆H₂₆N₆F₁₂P: C, 56.52; H, 2.68. Found: C, 56.57; H, 2.66.