反应详情

温度

50 °C

To a stirred solution of methyl 1-(4-((3-(azido(phenyl)methyl)phenoxy)methyl)-phenyl)cyclopropanecarboxylate (0.569 g, 1.375 mmol) in methanol (12.9 mL) and tetrahydrofuran (5.1 mL), was added 2M aqueous sodium hydroxide (12.9 mL). The reaction was stirred at 50° C. for 3 hours 30 minutes and then at room temperature for 16 hours. The reaction mixture was concentrated under reduced pressure, and the pH was adjusted to pH4 using 2M aqueous hydrochloric acid with stirring. The mixture was extracted with dichloromethane (×3), and the combined organic extracts washed with brine, dried (magnesium sulfate), filtered, and concentrated under reduced pressure to afford the title compound (0.552 g, quantitative yield). The material was used directly in the next step with no further purification

1. waitat room temperature for 16 hours
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. stirringwith stirring
4. extractionThe mixture was extracted with dichloromethane (×3)
5. washthe combined organic extracts washed with brine
6. dry with materialdried (magnesium sulfate)
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure