Compound 2-Cs

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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 CsC₈ (23 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 CsC₈ (23 mg, 0.102 mmol) was added slowly over several minutes (5-10 mg aliquots). The solution was stirred for an additional 30 minutes, during which time a dark brown solid precipitated from the solution Filtration allowed for isolation of this dark solid which was filtered once more with THF to separate the graphite, isolating pure [U(NDIPP)₄][Cs₂] (2-Cs) as a dark brown solid, after removal of the volatiles in vacuo. (Yield: 115 mg, 0.089 mmol, 89%). Crystals of 2-Cs were grown from a concentrated THF/toluene solution containing 2-Cs at -34 °C. ¹H NMR (300 MHz, C₆D₆, 25 ºC, TMS) δ = 1.53 (d, ³J(H,H) = 6Hz, 36H, iPrCH₃), 4.81 (sept, ³J(H,H) = 6 Hz, 6H, iPrCH), 4.97 (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 = 1.32 (d, ³J(H,H) = 6Hz, 36H), 4.59 (t, ³J(H,H) = 6 Hz, 3H, p-ArH), 4.77 (sept, ³J(H,H) = 6 Hz, 6H, iPrCH), 7.54 (d, ³J(H,H) = 6 Hz, 6H, m-ArH); ¹³C NMR (300 MHz, THFd₈, 25 ºC, TMS) δ = 26.15 (iPrCH), 26.61 (iPrCH₃), 117.42 (m-CH), 119.98 (p-CH), 148.92 (i-C), 163.74 (o-C); IR (KBr plate): = 3040 (w), 2954 (vs), 2864 (s), 1574(w), 1458 (s), 1398 (s), 1352 (w), 1318 (s), 1247 (vs), 1110 (w), 893 (w), 752 (s), 745 (s); analysis (calcd., found for C₆₄H₁₀₀N₄Cs₂O₄U): C (47.85, 47.99), H (5.69, 5.78), N (4.65, 4.38).