Bromine → HCID 86711541, compound

Participants

Reaction Steps

To a solution of 1-(4-cyano-benzyl)-4-oxo-1,4-dihydro-pyridine-3-carboxylic acid (preparation 12a, 2.57 g, 10.1 mmol) in glacial acetic acid (10 ml) is added bromine (2 mL). The reaction mixture is stirred for 6 days at room temperature and additional bromine (1 mL) is added on the first 2 days, respectively. The reaction mixture is evaporated under reduced pressure and co-evaporated with toluene twice. The remaining residue is purified by preparative reversed-phase HPLC (XBridge, gradient of methanol in water, 0.3% NH4OH, 60° C.). Yield: 566 mg (17% of theory); ESI mass spectrum: [M+H]+=333 (bromine isotope pattern); Retention time HPLC: 0.84 min (Z002—002).

Provenance & Evidence