反应详情

D8 (0.25 g, 0.824 mmol) and phosphorus (V) oxychloride (0.116 ml, 1.236 mmol) in DMF (5 ml) was heated in a sealed tube at 80° C. for 4 h. After cooling, the mixture was concentrated in vacuo. The crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 3% as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D9 (0.070 g, 26%).

1. temperatureAfter cooling
2. concentrationthe mixture was concentrated in vacuo
3. customThe crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 3% as eluent)
4. customThe desired fractions were collected
5. concentrationconcentrated in vacuo