Water → HCID 46829808, compound

Participants

Reaction Steps

To a solution of example 20 (71 mg; 0.13 mmol) in THF (4.5 mL) was added lithium hydroxide (16 mg; 0.67 mmol) (1.50 ml), followed by water (2 mL) and the resulting mixture was stirred at RT for 24 hours. The solution was diluted with NaOH (0.1 M) washed with Et2O and acidified to pH 1 with 1M HCl (1 M). The formed precipitate was filtered, washed with water and dried under high vacuum to give the title compound as an off-white solid (56 mg, 83%). 1H NMR (DMSO-d6) δ 12.97 (bs, 1H), 11.86 (bs, 1H), 8.45-8.41 (m, 1H), 8.37-8.36 (m, 1H), 8.31 (s, 1H), 7.85 (d, J=8.4 Hz, 1H), 7.20 (m, 1H), 7.06 (m, 1H), 3.90 (s, 1H), 3.15 (m, 1H), 2.97-2.93 (m, 1H), 2.64-2.57 (m, 1H), 1.80-1.76 (m, 2H), 1.63-1.29 (m, 4H), 0.78 (d, J=6 Hz, 3H). HPLC (Method A) Rt 5.43 min (Purity: 99.1%). LC/MS (method A): 501.3 (M+H)+.

Provenance & Evidence