Acetic Anhydride → HCID 59519434, compound

Participants

Reaction Steps

Acetic anhydride (0.95 mmol) is added to a solution of 5-chloro-4-(2-fluoro-4-iodophenylamino)-6-hydrazinylnicotinic acid (0.4 g, 0.95 mmol) and triethylamine (1.9 mmol) in DCM (10 ml) at 0° C. The reaction mixture is warmed to room temperature, stirred for an additional 10 min and POCl3 (0.95 mmol) is added. After stirring overnight at room temperature the mixture is refluxed for 3 days. It was diluted with EtOAc and NaHCO3 and stirred for 20 min. The organic layer is washed with H2O, brine, dried with Na2SO4 and concentrated under reduced pressure. The crude product is purified by column chromatography.

Provenance & Evidence