Triphenylphosphine → HCID 67972521, compound

Participants

Reaction Steps

A mixture of the title compound from Step F above (1.00 g, 1.69 mmol) and palladium acetate Pd(OAc)2 (0.064 g, 0.28 mmol) in ethanol (15 ml) was degassed and flushed with N2, and then triphenylphosphine (0.298 g, 1.137 mmol) was added. The reaction mixture was refluxed overnight. After removal of the solvent, the residue was purified by column chromatography (0-20% then 20% ethyl acetate in hexanes). 0.50 g (50%) of the title compound was obtained. 1H NMR (CDCl3, 400 MHz): δ8.14 (d, J=8.6 Hz, 2H), 7.53-7.28 (m, 12H), 5.13 (s, 2H), 4.97 (d, J=9.4 Hz, 1H), 4.86 (s, 1H), 4.06 (s, 3H), 3.85 (s, 2H), 2.77-2.64 (m, 2H), 2.07 (m, 1H), 1.85-1.79 (m, 2H), 1.05 (s, 9H), 0.19 (s, 3H), 0.00 (s, 3H). MS: m/z (ESI) 590 (M+1).

Provenance & Evidence