Bromine → HCID 15896326, compound

Participants

Reaction Steps

A solution of bromine (78.3 μl, 1.48 mmol) in acetic acid (6 ml) was added dropwise to a stirred solution of 6-(4-fluorophenyl)-4,5-dihydro-5-(4-pyridyl)-2H-pyridazin-3-one (314 mg, 1.17 mmol) in acetic acid (4.6 ml) at room temperature. After 2 h at room temperature, more bromine (41.7 μl, 0.78 mmol) in acetic acid (3.2 ml) was added to the turbid mixture. A gum precipitated. After 30 minutes, it was evaporated and co-evaporated with toluene. Residual acid was neutralized with methanolic 2N ammonia followed by evaporation. The resulting product was purified on a column of silica gel (3-5% methanol/dichloromethane) to provide the title compound as a solid. MS (m/z): 268.1 (M+H)+; C15H16FN3O requir. 267.3.

Provenance & Evidence