Lithium Hydroxide → HCID 75202188, compound

Participants

Reaction Steps

Lithium hydroxide (0.114 g, 2.72 mmol) was added to a solution of 14B2 (0.3 g, 0.543 mmol) in 6 mL of ethanol-water (3:1) mixture, and the mixture was stirred at room temperature for 5 h. After the solvent was removed in vacuo, the residue was diluted with water. The aqueous layer was acidified with addition of saturated citric acid solution until pH 3 was attained. The resulting solution was cooled to 0° C., and solids obtained were filtered off and dried under vacuum to afford the title compound (0.2 g, 88%) as a solid. 1H NMR (300 MHz, DMSO-d6) δ 12.47 (s, 1H), 10.47 (s, 1H), 8.98 (dd, J1=1.9 Hz, J2=7.7 Hz, 2H), 8.53 (dd, J1=2.1 Hz, J2=8.7 Hz, 1H), 8.46 (s, 1H), 8.10-7.93 (m, 3H), 7.88 (d, J=8.7 Hz, 1H), 3.26-2.92 (m, 3H), 2.88-2.64 (m, 2H), 2.58-2.42 (m, 2H), 2.17 (m, 1H). ESI-MS m/z: 525 (M+H)+; HPLC purity: 97%.

Provenance & Evidence