反应详情

温度

70 °C

To a solution of the product from Step B above (0.18 g, 0.33 mmol) in pyridine (9.0 mL) was added phosphorus oxychloride (0.25 g, 1.65 mmol). The mixture was heated at 70° C. for 7 hours, and stirred at 35° C. overnight, then concentrated to dryness under reduced pressure. The residue was dissolved in EtOAc and washed with saturated NaHCO3, water and brine. The organic layer was separated and dried over Na2SO4. The crude product was purified on a silica gel column using a gradient of 0-50% ethyl acetate in hexanes to give the title compound as light brown solid. LC/MS m/z=526.1[M+H]+.

1. concentrationconcentrated to dryness under reduced pressure
2. dissolutionThe residue was dissolved in EtOAc
3. washwashed with saturated NaHCO3, water and brine
4. customThe organic layer was separated
5. dry with materialdried over Na2SO4
6. customThe crude product was purified on a silica gel column