反应详情

To a solution of the intermediate from Step F (7.1 g, 22.42 mmol) in 1,2-dichloroethane (30 mL) was added phosphorous oxychloride (10.45 mL, 112 mmol). The resulting mixture was refluxed for 18 hours. The reaction mixture was cooled to room temperature and concentrated. The residue was partitioned between water and ethyl acetate. The aqueous layer was neutralized with solid sodium bicarbonate and then extracted with ethyl acetate (3×). The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography using a hexanes/EtOAc gradient to give a light yellow solid. m/z=298.9 (M+H).

1. temperatureThe resulting mixture was refluxed for 18 hours
2. concentrationconcentrated
3. customThe residue was partitioned between water and ethyl acetate
4. extractionextracted with ethyl acetate (3×)
5. washThe organic layer was washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was purified by silica gel chromatography
10. customto give a light yellow solid