Hydrochloric Acid → HCID 9870752, compound

Participants

Reaction Steps

LiOH.H2O (120 mg, 2.9 mmol) was added to a solution of the compound of Example 1 (0.98 g, 1.9 mmol) in THF (10 ml) and water (5 ml) and the reaction stirred at room temperature for 1.5 h, then acidified to pH1 with 10% hydrochloric acid and extracted with DCM (2×25 ml). The combined organic layers were dried (MgSO4) and the solvent evaporated in vacuo to give a white foam that was triturated with DCM/Et2O to give the title compound as a white solid (0.52 g, 54%). δH (DMSO d6) 9.09 (1H, br s, NH), 7.58-7.44 (3H, m, Ar—H), 6.98 (2H, d, J 8.4 Hz, Ar—H), 6.65 (2H, d, J 8.4 Hz, Ar—H), 5.20 (2H, s, CH2OAr), 3.69 (6H, s, OMe), 3.69 (1H, m, CHCH2) and 3.05 (2H, m, CHCH2). m/z (ESI, 60V) 504, 506 (MH+).

Provenance & Evidence