反应详情

温度

50 °C

Triphenylphosphine (0.74 g, 2.8 mmol) was dissolved in tetrahydrofuran (0.94 mL, 1.1 mmol) and diisopropyl azodicarboxylate (0.35 mL, 1.8 mmol), 3-methoxypropan-1-ol (0.14 mL, 1.5 mmol) and 6-fluoro-2-methylquinolin-8-ol (0.20 g, 1.1 mmol) were added. The vessel was sealed and the mixture was stirred at 50° C. for 12 hours. The cooled reaction mixture was diluted with water (10 mL) and extracted with dichloromethane (2×20 mL). The combined organic extracts were dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by normal phase chromatography on silica gel (10-50% ethyl acetate/hexanes) to provide the title compound (0.22 g, 77%).

1. customThe vessel was sealed
2. customThe cooled reaction mixture
3. extractionextracted with dichloromethane (2×20 mL)
4. dry with materialThe combined organic extracts were dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by normal phase chromatography on silica gel (10-50% ethyl acetate/hexanes)