反应详情

To a solution of 3-(3-azidopropyl)-5-chloro-1H-indole (0.299 g; 1.27 mmol) in tetrahydrofuran (9 mL) were added triphenylphosphine (0.354 g; 1.34 mmol) and water (0.6 mL). The reaction mixture was stirred at room temperature for 22 hours and was then evaporated to dryness. The residue was dissolved in dichloromethane (10 mL) and 10 mL of 6N hydrochloric acid were added. After separation, the aqueous layer was further extracted with dichloromethane (2×10 mL) and the pH was adjusted to 14 with a solution of sodium hydroxide 6N. This basic solution was extracted with dichloromethane (3×20 mL) and the combined organic layer was dried over magnesium sulfate, and evaporated to afford 0.089 g (34%) of 3-(5-chloro-1H-indol-3-yl)propan-1-amine as a white solid.

1. customwas then evaporated to dryness
2. dissolutionThe residue was dissolved in dichloromethane (10 mL)
3. addition10 mL of 6N hydrochloric acid were added
4. customAfter separation
5. extractionthe aqueous layer was further extracted with dichloromethane (2×10 mL)
6. extractionThis basic solution was extracted with dichloromethane (3×20 mL)
7. dry with materialthe combined organic layer was dried over magnesium sulfate
8. customevaporated