Compound 2-K

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Compound data: CIF

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

In a 20 mL scintillation vial, a stirring Et₂O solution (~10 mL) of 1 (100 mg, 0.102 mmol) was treated with a single equivalent of KC₈ (14 mg, 0.102 mmol) resulting in a slight darkening of the solution. After 5 minutes of vigorous stirring, a single equivalent of N₃DIPP (20 mg, 0.102 mmol) was added to the solution dropwise, with vigorous release of N₂ observed. After 5 minutes of stirring, a second equivalent of KC₈ (14 mg, 0.102 mmol) was added slowly over several minutes (5-10 mg aliquots), again showing effervescence of N₂. After stirring for an additional 30 minutes, filtration and removal of volatiles in vacuo produced a dark brown solid identified as [U(NDIPP)₄][K₂] (2-K) (105 mg, 0.097 mmol, 96%). Crystals of 2-K were grown from a concentrated THF/pentane solution containing 2-K at -34 °C. ¹H NMR (300 MHz, C₆D₆, 25 ºC, TMS) δ = 1.49 (d, ³J(H,H) = 6Hz, 36H, iPrCH₃), 4.66 (sept, ³J(H,H) = 6 Hz, 6H, iPrCH), 5.07 (t, ³J(H,H) = 6 Hz, 3H, p-ArH), , 7.79 (d, ³J(H,H) = 6 Hz, 6H, m-ArH); ¹³C NMR (75 MHz, C₆D_6, 25 ºC, TMS) δ = 25.71 (iPrC H), 26.04 (iPrCH₃), 117.36 (m-CH), 121.29 (p-CH), 149.29 (i-C), 161.24 (o-C); IR (KBr plate): = 3037 (w), 2954 (vs), 2864 (s), 1575(w), 1459 (s), 1400 (s), 1354 (w), 1314 (s), 1243 (vs), 1134 (w), 895 (w), 747 (s); analysis (calcd., found for C₆₄H₁₀₀N₄K₂O₄U): C (56.71, 56.71), H (6.74, 6.67), N (5.51, 5.24).