Compound 4

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InChIKey NOXVWBLCEKOJBW-UHFFFAOYSA-N

Compound data: CIF

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

A C₆D₆ solution (0.5 mL) of 3b (20 mg, 0.014 mmol) was stirred at 80 °C under H₂ (1 atm) for 1 day. After the solvent was removed in vacuo, the residue was taken up in a minimal amount of Et₂O and recrystallized at –35 °C to give 4 (16 mg, 0.011 mmol, 71%) as colorless crystals suitable for X-ray analysis. ¹H NMR (300 MHz, C₆D₆, rt): δ 5.12 (brs, 7H, Y-H-Y), 2.54 (s, 24H, C₅Me₄SiMe₃), 2.33 (s, 24H, C₅Me₄SiMe₃), 2.06 (s, 15H, C₅Me₅), 0.55 (s, 36H, C₅Me₄SiMe₃), -3.09 (brs, 5H, W-H-Y), -4.72 (brs, 1H, W-H). ¹H NMR (300 MHz, toluene-d₈, -40 °C): δ 5.26 (qt, J_HY = 17.7 Hz, 6H, Y-H-Y), 3.62 (m, 1H, Y-H-Y), 2.58 (s, 24H, C₅Me₄SiMe₃), 2.37 (s, 24H, C₅Me₄SiMe₃), 2.04 (s, 15H, C₅Me₅), 0.59 (s, 36H, C₅Me₄SiMe₃), -3.14 (d, J_HH = 9.9 Hz, J_HW satellite = 44.1 Hz, 5H, W-H-Y), -4.62 (brs, 1H, W-H). ¹³C NMR (75 MHz, toluene-d₈, rt): δ 128.4 (s, C₅Me₄SiMe₃), 124.9 (s, C₅Me₄SiMe₃), 115.2 (s, C₅Me₄SiMe₃), 102.2 (s, C₅Me₅), 16.8, 13.0, 12.8 (s, C₅Me₅ or C₅Me₄SiMe₃), 2.9 (s, C₅Me₄SiMe₃). IR (Nujol mull): ν 2951 (s), 2922 (s), 2853 (s), 1751 (w), 1458 (m), 1246 (m), 847 (m), 835 (m) cm^-1. Anal. calcd for: C₅₈H₁₁₂WSi₄Y₄: C, 47.68; H, 7.67. Found: C, 48.78; H, 7.74.