反应详情

温度

100 °C

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%).

1. temperatureto cool to room temperature
2. concentrationconcentrated
3. temperatureIt was cooled with an acetone-CO2 bath
4. additionEtOAc and ice were subsequently added
5. customThe organic phase was decanted
6. washwashed with saturated NaHCO3
7. dry with materialdried over Na2SO4
8. concentrationconcentrated to dryness
9. customThe crude obtained
10. customwas purified by chromatography on silica gel
11. temperatureof increasing polarity