Lithium Hydroxide → HCID 59050119, compound

Participants

Reaction Conditions

Reaction Steps

The compound of Example 17 (22.0 mg, 0.04 mmol, 1 equiv) was dissolved in THF/MeOH/H2O 3:1:1 (1 mL) and cooled to 0° C. Solid lithium hydroxide (5.3 mg, 0.22 mol, 5 equiv) was added and the reaction mixture was stirred for two hours at 0° C. The solvents were removed under reduced pressure and the residue was taken up with H2O (2 mL). The resulting solution was acidified with 0.1 N HCl to pH 3 and stirred for 30 min., while a white precipitate was formed. The precipitated title compound was isolated by filtration and dried under vacuum. Yield 15.0 mg, 70.2%. 1H NMR (DMSO, 200 MHz) δ 10.45 (brs, 1H); 9.65 (s, 1H); 8.61 (s, 1H); 7.90-7.71 (m, 1H); 7.65-7.55 (m, 1H); 7.59-7.43 (m, 1H); 7.39-7.17 (m, 3H); 7.02 (d, 1H); 6.84 (d, 1H); 4.49-4.38 (m, 1H); 4.30-4.19 (m, 1H); 4.0 (q, 2H); 3.19-3.02 (m, 1H); 1.17 (t, 3H); 0.85-0.65 (m, 4H). MS (EI) 502 (M+Na), 480 (M+H), 321.

Provenance & Evidence