Sodium Hydroxide → HCID 178433648, compound

Participants

Reaction Steps

To a solution of sodium hydroxide (0.075 g, 1.88 mmol) in methanol (10 ml) was added the product of Example 105 (0.1 g, 0.42 mmol) and the mixture stirred for 18 hours. The solvent was evaporated in vacuo and the residue taken up in water and adjusted to pH 6 with 1N HCl. The yellow precipitate was extracted into 10% methanol/CH2Cl2 and the organic phase separated, dried, filtered and evaporated to give a yellow solid. Recrystallisation from MeOH/CH2Cl2/EtOAc afforded the title compound as a yellow solid (0.082 g, 60.5%). 1H NMR (360 MHz, DMSO-d6) δ12.22 (1H, br s), 8.44 (1H, s), 8.23 (2H, d, J 8.9 Hz), 7.46 (2H, d, J 8.9 Hz), 4.54 (1H, t, J 5.3 Hz), 3.44 (2H, dt, J 5.5, J 6.2 Hz), 2.71 (2H, t, J 7.2 Hz), 2.35 (3H, s), 1.78 (2H, t, J 7.2 Hz); MS (ES+) m/z 318/320 [MH]+.

Provenance & Evidence