Compound 7a

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InChIKey IJZQVFAGCUZTAU-UHFFFAOYSA-M

Compound data: CIF

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

To a solution of 2a (56.1 mg. 0.050 mmol) in THF (5 mL) was added HBF₄·OEt₂ (27 μL, 0.20 mmol) and stirred at room temperature for 24 h. The resultant dark green solution was treated with pyridine (40 μL, 0.50 mmol) and stirred at room temperature for additional 2 h. The volatile components were removed under vacuum. The residue was extracted with benzene−THF (5 mL−3 mL), and slow addition of Et₂O (15 mL) afforded green crystals, which were collected by filtration and dried in vacuo to obtain 7a·0.5C₆H₆ as a green-brown crystalline solid (35.3 mg, 0.047 mmol, 47% yield). ¹H NMR (THF-d₈) δ 9.38 (d, J = 5.7 Hz, ArH, 2H), 7.77−7.75 (br, ArH, 2H), 7.64 (d, J = 7.3 Hz, ArH, 2H), 7.54 (t, J = 7.3 Hz, ArH, 1H), 7.33−7.28 (m, ArH and C₆H₆, 4H), 6.82 (br, NNH₂, 2H) 3.96−3.75 (m, CH₂P^tBu₂, 4H), 1.21 (pseudo t, CH₂P^tBu₂, 18H), 1.10 (pseudo t, CH₂P^tBu₂, 18H). ³¹P{¹H} NMR (THF-d₈) δ 77.6 (d, ²J_PF = 29.3 Hz, PNP). IR (KBr, cm⁻¹) 3378, 3277 (s, ν_NH). Anal Calcd for C₃₁H₅₃BF₅MoN₄P₂: C, 49.95; H, 7.17; N, 7.52. Found: C, 49.56; H, 7.10; N, 7.84.