Triphenylphosphine → HCID 86605359, compound

Participants

Reaction Steps

A mixture of 38 (805 mg, 1.15 mmol) in THF (8 mL) and water (1.6 mL) is treated with triphenylphosphine (640 mg, 2.44 mmol) and stirred at room temperature for 14 h. The reaction mixture is concentrated and purified on silica gel column using chloroform:CMA-80 (1:0 to 1:1) as eluent to give 660 mg (85%) as a white solid: 1H NMR (DMSO-d6): δ 8.09 (s, 1H), 7.72 (s, 1H), 7.17-7.00 (m, 13H), 6.67 (d, J=9.0 Hz, 2H), 4.70-4.59 (m, 1H), 4.28-4.16 (m, 2H), 3.95 (t, J=9.2 Hz, 1H), 3.68-3.45 (m, 3H), 3.54 (s, 3H), 2.29-2.05 (m, 2H), 1.93-1.60 (m, 4H), 0.96-0.91 (m, 6H), 0.84 (d, J=6.1 Hz, 6H). IR (neat, cm−1) 3414, 3020, 1605, 1511 and 1216. Anal. Calcd for C36H45N6O5P.1.5 H2O: C, 61.79; H, 6.91; N, 12.01. Found: C, 61.70; H, 6.63; N, 12.07.

Provenance & Evidence