Compound 2-Rb

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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 RbC₈ (18 mg, 0.102 mmol) resulting in 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. After 5 minutes of stirring, a second equivalent of RbC₈ (18 mg, 0.102 mmol) was added slowly over several minutes (5-10 mg aliquots). After stirring for an additional 30 minutes, filtration and removal of volatiles in vacuo produced a dark brown solid identified as [U(NDIPP)₄][Rb₂] (2-Rb) (100 mg, 0.085 mmol, 84%). Crystals of 2-Rb were grown from a concentrated THF solution containing 2-Rb at -34 °C. ¹H NMR (300 MHz, C₆D₆, 25 ºC, TMS) δ = 1.52 (d, ³J(H,H) = 6Hz, 36H, iPrCH₃), 4.73 (sept, ³J(H,H) = 6 Hz, 6H, iPrCH), 5.02 (t, ³J(H,H) = 6 Hz, 3H, p-ArH), , 7.81 (d, ³J(H,H) = 6 Hz, 6H, m-ArH); ¹H NMR (300 MHz, THFd₈, 25 ºC, TMS) δ = 1.30 (d, ³J(H,H) = 6Hz, 36H, iPrCH₃), 4.59 (t, ³J(H,H) = 6 Hz, 3H, p-ArH), 4.73 (sept, ³J(H,H) = 6 Hz, 6H, iPrCH), 7.53 (d, ³J(H,H) = 6 Hz, 6H, m-ArH); ¹³C NMR (300 MHz, THFd₈, 25 ºC, TMS) δ = 26.15 (iPrCH), 26.64 (iPrCH₃), 117.22 (m-CH), 120.31 (p-CH), 148.91 (i-C), 163.39 (o-C); IR (KBr plate): = 3039 (w), 2954 (vs), 2863 (s), 1573(w), 1457 (s), 1398 (s), 1352 (w), 1318 (s), 1245 (vs), 1110 (w), 892 (w), 752 (s), 745 (s); analysis (calcd., found for C₆₄H₁₀₀N₄Rb₂O₄U): C (51.94, 51.78), H (6.17, 6.16), N (5.05, 5.09).