Water → HCID 67229016, compound

Participants

Reaction Steps

Polymer supported triphenylphosphine (9.5 g, 28 mmol) was added to the product of Example 20B (4.6 g, 14 mmol) in THF (100 mL) containing 1.3 g (71 mmol) H2O. The mixture was stirred for 48 hours at ambient temperature, then diluted with THF and filtered through a pad of celite. The filter cake was washed with 3 solvents systems sequentially comprising 100% CH3OH, 1:1 CH3OH:CH2Cl2, and 100% CH2Cl2. The filtrate was concentrated under reduced pressure to provide 3.5 g (83%) of the title compound. 1H NMR (DMSO-d6) δ 8.81 (s, 1H), 7.45-7.30 (m, 5H), 7.13 (d, J=8 Hz, 1H), 7.05 (t, J=7 Hz, 1H), 6.90 (d, J=7 Hz, 1H), 5.12 (s, 2H), 3.00-2.65 (m, 4H), 2.23 (m, 1H), 1.84 (m, 1H), 1.59 (br s, 2H), 1.37 (m, 1H); MS (ESI+) m/z 297 (M+H)+.

Provenance & Evidence