Ethyl Acetate → HCID 59495659, compound

Participants

Reaction Steps

To a solution of example 117 (1 860 mg; 3.69 mmol) in MeOH (40 mL), sodium hydroxide (3.69 mL; 5 M; 18.5 mmol) in H2O was added. The reaction was stirred at RT for 1 h. EtOAc was added and the organic phase washed 3 times with HCl 1M. The organic phase was dried over MgSO4, filtered off and concentrated to afford the title compound as a white powder (1490.0 mg, 82%). 1H NMR: (DMSO-d6, 300 MHz) δ 8.58 (m, 1H), 8.33 (brs, 1H), 8.18 (dd, J=1.7 Hz, 8 Hz, 1H), 8.03 (dd, J=1.7 Hz, 8 Hz, 1H), 7.95 (d, J=10.6 Hz, 1H), 7.84 (t, J=7.6 Hz, 1H), 7.44 (d, J=7.9 Hz, 1H), 7.40-7.22 (m, 3H), 7.15 (m, 1H), 4.23 (d, J=12.9 Hz, 1H), 4.17 (d, J=12.9 Hz, 1H), 3.49 (m, 2H), 3.25 (s, 3H), 2.53 (m, 2H), 2.04 (s, 3H). LC/MS (Method B): 490.3 (M+H)+ 488.4 (M−H)−. HPLC (Method A) Rt: 4.83 min (purity: 99.7%).

Provenance & Evidence