Water → HCID 56962847, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred solution of Compound (11) (250 mg, 0.45 mmol) in MeOH (20 mL) was added ammonium fluoride (166 mg, 4.5 mmol) and water (5 mL). The reaction mixture was heated to 60° C. for 5 h (monitored by TLC and LCMS). MeOH was removed in vacuo and the residue was diluted with water. The resulting precipitate was filtered, washed with ethanol and dried in vacuo at 40° C. to give Compound (12) (65 mg, 33%). ESI-MS m/z calculated for [M+Na]+: 459.11; found: 459.11; 1H NMR (400 MHz, d6-DMSO) δ 8.65 (s, 1H), 7.77 (s, 1H), 7.65-7.52 (m, 2H), 7.46-7.32 (m, 2H), 7.15 (s, 1H), 4.80-4.70 (m, 1H), 3.92 (s, 3H), 3.78-3.39 (m, 4H), 3.08 (s, 3H), 2.88-2.77 (m, 3H).

Provenance & Evidence