反应详情

温度

90 °C

70 mL of phosphorylchloride were added to 14.9 g of 1a and the mixture was heated at 90° C. for 2 hours. Excess of phosphorylchloride was evaporated, water was added, followed by aqueous 2N NaOH until pH 9 and the mixture was extracted with dichloromethane. The dichloromethane extract was washed with brine, dried (MgSO4) and concentrated. The residue was chromatographed on silica gel (toluene/ethyl acetate=4/1) giving 10.1 g of 1b. M.p.=102.7-103.7° C.

1. customExcess of phosphorylchloride was evaporated
2. additionwater was added
3. extractionthe mixture was extracted with dichloromethane
4. extractionThe dichloromethane extract
5. washwas washed with brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customThe residue was chromatographed on silica gel (toluene/ethyl acetate=4/1)