Hydrochloric Acid → HCID 9795059, compound

Participants

Reaction Steps

To a stirred solution of 142 (0.552 g, 2 mmol) in pyridine (4 mL), 1N NaOH (4 mL, 4 mmol) was added. The resulting mixture was stirred for 4 h, then diluted with water (50 mL) and acidified with 2N HCl to pH 2. The precipitated crude product was washed with water, dried on a filter and washed with ether (5×5 mL) to give 0.365 g (72%) of the title compound as an orange solid: mp 294°-296° C. (from EtOH); IR (KBr) 3104, 3048, 2231, 1675, 1623, 1453, 1399 and 1176 cm-1 ; 1H NMR (DMSO-d6) δ7.54 (s, 1H), 8.25 (s, 1H), 12.20 (s, 1H, N--H). HPLC: 95%; HRMS Calcd for C9H3N3O2Cl2 : 254.9602. Found: 254.9604.

Provenance & Evidence