Phosphorus oxychloride → HCID 86606795, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 6-(4-fluorophenyl)-2-(hydroxy)-5-(2-methylsulfanylpyrimidin-4-yl)pyridin-3-carbonitrile (48.84 g, 144.6 mmol, obtained in reference example 21), POCl3 (166 mL, 1.8 mol) and DMF (2.2 mL) was heated to 100° C. for 2 h. It was allowed to cool to room temperature and concentrated. It was cooled with an acetone-CO2 bath and EtOAc and ice were subsequently added. The organic phase was decanted, washed with saturated NaHCO3, dried over Na2SO4 and concentrated to dryness. The crude obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity, to afford 31.00 g of the title compound (yield: 60%).

Provenance & Evidence