反应详情

A mixture of PCl5 (16.6 g, 80 mmol) in dichloromethane (500 mL) was added dropwise to a suspension of Example 96A (8.6 g, 40 mmol) in dichloromethane (80 mL). The resulting mixture was heated to reflux for 20 hours, cooled to room temperature, and concentrated. The residue was dissolved in a minimal amount of dichloromethane and filtered through a plug of silica gel. The plug was washed with dichloromethane and the filtrate was concentrated. The concentrate was recrystallized from dichloromethane/hexanes to provide 5.4 g (57% yield) of the desired product. Rf=0.7 (5% methanol/dichloromethane).

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 20 hours
3. concentrationconcentrated
4. dissolutionThe residue was dissolved in a minimal amount of dichloromethane
5. filtrationfiltered through a plug of silica gel
6. washThe plug was washed with dichloromethane
7. concentrationthe filtrate was concentrated
8. customThe concentrate was recrystallized from dichloromethane/hexanes