Water → HCID 70913731, compound

Participants

Reaction Steps

A solution of compound 45 (720 mg, 1.58 mmol) and NaOH (5.0 g, 127 mmol) in a mixture of EtOH (15 mL) and H2O (10 mL) was stirred at reflux for 3 d, cooled to rt, concentrated and redissolved in H2O (30 mL) and acidified with 1N HCl solution to pH=6. The formed solid was collected by filtration, washed with EA and dried in vacuum to give the title compound 46 (750 mg, 100%) as a white solid. 1H-NMR (DMSO-d6, 400 MHz) δ: 0.63-0.65 (2H, m), 0.90-0.95 (3H, m), 1.22-1.25 (3H, m), 1.30 (9H, s), 1.45 (3H, m), 1.49 (6H, s), 2.43 (3H, s), 3.76 (2H, d, J=6.8 Hz), 6.29 (1H, s), 6.92 (2H, s), 7.08 (1H, s), 7.23 (1H, s), 7.34 (1H, s), 12.38 (1H, s). MS Calcd.: 474; MS Found: 475 (M+1).

Provenance & Evidence