反应详情

The compound (44.83 g, 0.264 mol) obtained in Example 1, triethyl phosphite (53.21 g, 0.320 mol), potassium iodide (39.4 g, 0.237 mol) and acetonitrile (224 mL) were charged and stirred under reflux for 4 hrs. The reaction mixture was allowed to return to room temperature, and water (336 mL) was added. The mixture was concentrated under reduced pressure, and the residue (315 g) was stirred at room temperature for 1 hr. and under ice-cooling for 1 hr. The crystals were collected by filtration, washed with cold water (20 mL) and dried in vacuo at 40° C. for 7 hrs. to give the title compound (66.79 g, yield 93.2%) as slightly yellow crystals.

1. temperatureunder reflux for 4 hrs
2. customto return to room temperature
3. concentrationThe mixture was concentrated under reduced pressure
4. stirringthe residue (315 g) was stirred at room temperature for 1 hr
5. temperatureand under ice-cooling for 1 hr
6. filtrationThe crystals were collected by filtration
7. washwashed with cold water (20 mL)
8. customdried in vacuo at 40° C. for 7 hrs