反应详情

温度

100 °C

To the product of Step B (1.5 g) was added POCl3 (5 mL). The reaction was heated to 100° C. for 17 hours. After cooling to room temperature the excess POCl3 was removed in vacuo before the residue was dissolved in EtOAc and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel eluted with 10% EtOAc in hexane affording the title compound. HPLC/MS: 358.9 (M+1), 360.9 (M+3); Rt=4.07 min.

1. customwas removed in vacuo before the residue
2. dissolutionwas dissolved in EtOAc
3. washwashed with saturated aqueous NaHCO3 solution
4. concentrationThe solution was concentrated
5. custompurified via flash chromatography on silica gel
6. washeluted with 10% EtOAc in hexane affording the title compound