反应详情

温度

70 °C

Sodium iodide (1.5 g) was added to a DMF solution (20 ml) of 2-(3-bromopropoxy)tetrahydropyran (0.85 ml). The mixture was stirred at 70° C. for 7 hours. The reaction mixture was cooled to room temperature. (2-Pyridin-3-yl-ethyl)-pyridin-4-ylmethyl-amine (1.28 g), and N-ethyldiisopropylamine (1.3 ml) were added thereto. The mixture was stirred at room temperature overnight. Water was added to the reaction mixture, followed by extraction using ethyl acetate. The organic layer was washed with water and then saturated saline, and dried with anhydrous sodium sulfate. After condensation under reduced pressure, the residue was purified by silica gel column chromatography (ethyl acetate:methanol=20:1→4:1). The purified product was condensed under reduced pressure to give the title compound (236 mg) as a colorless oily matter.

1. temperatureThe reaction mixture was cooled to room temperature
2. stirringThe mixture was stirred at room temperature overnight
3. extractionfollowed by extraction
4. washThe organic layer was washed with water
5. dry with materialsaturated saline, and dried with anhydrous sodium sulfate
6. customAfter condensation under reduced pressure
7. customthe residue was purified by silica gel column chromatography (ethyl acetate:methanol=20:1→4:1)
8. customcondensed under reduced pressure