Triphenylphosphine → HCID 22498670, compound

Participants

Reaction Steps

4-Oxo-1,4-dihydropyrido[2,3-c]pyridazine-3-carboxylic acid ethyl ester—3-(2-Chloropyridin-3-yl)-2-diazo-3-oxopropionic acid ethyl ester (5 g) in diisopropyl ether (150 ml) was treated with triphenylphosphine (5.7 g) and stirred at ambient temperature for 18 hours. The resulting solid was filtered off and dried in vacuo then treated with methanol (250 ml) and water (50 ml) and heated under reflux for 2 hours. The methanol was distilled off and the resulting aqueous extracted with EtOAc. The organic was dried and evaporated. Chromatography (EtOAc/hexane) gave title compound (3.2 g). MS (−ve ion chemical ionisation) m/z 218 ([M−H]−, 100%).

Provenance & Evidence