Trifluoroacetic acid → HCID 11961296, compound

Participants

Reaction Conditions

Reaction Steps

To a stirring solution of 2 (0.77 g, 2.24 mmol) in CH2Cl2 (25 mL) at 0° C., was added, drop wise, TFA over 15 min. The pale yellow, reaction was stirred at 0° C. for 1 h then allowed to stand at RT for 15 min. The reaction was concentrated to a viscous oil, redissolved in CH2Cl2 (20 mL) and reconcentrated to a gummy solid. The crude product was crystallized from ether/hexanes to afford the title compound (3) as a white solid (0.30 g, 41%). 1H NMR (300 MHz, DMSO-d6): δ 1.59 (s, 8H), 2.29 (br s, 4H), 6.52 (d, J=16 Hz, 1H), 7.15-7.39 (m, 7H), 7.59 (d, J=16 Hz, 1H), 7.66 (d, J=8.3 Hz, 2H), 12.41 (s, 1H). LRMS (APCI): m/z 433 (M+H)+. Anal. Calcd for C23H24O2: C, 83.07; H, 7.30. Found: C, 82.73; H, 7.25.

Provenance & Evidence