反应详情

温度

100 °C

A mixture of 4-hydroxy-1-(4-(methylsulfonyl)phenyl)pyridin-2(1H)-one (106.1 mg, 0.4 mmol) and phosphorous oxybromide (573.4 mg, 2 0 mmol, Alfa Aesar) was heated at 100° C. for 45 min and then cooed to room temperature. To the above residue was added saturated NaHCO3 aqueous solution at 0° C. followed by extraction with CH2Cl2 (3×). The combined extracts were washed with saturated NaHCO3 aqueous solution and brine, dried (Na2SO4) and evaporated. The residual was purified by flash chromatography (0 to 100% EtOAc/hexanes) to yield 60.7 mg (46%) of the product as a yellow solid. MS (ESI) 328 (M+H).

1. customcooed to room temperature
2. extractionfollowed by extraction with CH2Cl2 (3×)
3. washThe combined extracts were washed with saturated NaHCO3 aqueous solution and brine
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customThe residual was purified by flash chromatography (0 to 100% EtOAc/hexanes)