反应详情

A solution containing the compound from Step A (300 mg, 0.50 mmol), the N,N-diethylaniline (1.2 mL) and freshly distilled phosphorus chloride (24 mL) was stirred at reflux for 1 hour. The reaction mixture was evaporated to dryness. Dichloromethane was added to the residue and the organic layer poured over cracked ice/water. The aqueous layer was extracted with dichloromethane. The organic layer was washed with sodium hydrogenocarbonate 5%, water and was evaporated to dryness. The crude product was purified on silica gel using diethyl ether/petrol ether (1/1) as eluant to give the title compound (295 mg) as a white powder.

1. temperatureat reflux for 1 hour
2. customThe reaction mixture was evaporated to dryness
3. additionDichloromethane was added to the residue
4. additionthe organic layer poured over cracked ice/water
5. extractionThe aqueous layer was extracted with dichloromethane
6. washThe organic layer was washed with sodium hydrogenocarbonate 5%, water
7. customwas evaporated to dryness
8. customThe crude product was purified on silica gel