Phosphorus oxychloride → HCID 58961588, compound

Participants

Reaction Steps

To a dried round bottom flask fitted with a condenser was added methyl 6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)-2-oxo-1,2-dihydropyridine-3-carboxylate from Step A of Example 51 (1.50 g; 3.67 mmol) and excess phosphorous oxychloride (4 mL). The reaction mixture was heated to reflux for 16 hours. The reaction mixture was allowed to cool to room temperature, and the volatiles were removed in vacuo. The residue was redissolved in methylene chloride and washed with saturated NaHCO3 solution (2×), water, brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification was done by MPLC (silica gel; 0-10% ethyl acetate:hexane) to afford the desired product: m/e=428 (M+2) Rt=4.42 min on LCMS.

Provenance & Evidence