HCID 68648142, compound → HCID 136174013, compound

Participants

Reaction Steps

The product from step C (284 mg, 0.71 mmol) was heated to 60° C. in a mixture of TFA (5 mL) and water (1 mL) for 1 h. Upon cooling the reaction mixture was concentrated and partitioned between ethyl acetate and saturated sodium carbonate solution. The solid that formed at the solvent interface was removed by filtration and dried under vacuum to provide the pure title compound (63 mg, 33%) as a white solid: 1H NMR (500 MHz, DMSO-d6) δ 11.02 (s, 1H), 8.40 (s, 1H), 8.17 (s, 1H), 7.89 (d, J=9.9 Hz, 1H), 7.84 (s, 1H), 7.15 (d, J=9.9 Hz, 1H), 3.79 (t, J=3.9 Hz, 4H), 3.52 (t, J=4.3 Hz, 4H); 13C NMR (125 MHz, DMSO-d6) δ 155.2, 136.1, 135.8, 128.4, 125.8, 125.1, 121.8, 109.2, 108.6, 65.6, 46.0; HPLC tR=13.6 min (Luna), >99%; ES-MS: (M+H)=271 m/z.

Provenance & Evidence