反应详情

温度

23 °C

A solution of 3-(2-(4-(pyridin-2-ylamino)phenoxy)pyridin-3-yl)cyclopent-2-enol (190 mg, 0.550 mmol) in Tetrahydrofuran (10 mL) was treated with palladium, 10% wt. on activated carbon (58.5 mg, 0.055 mmol, 0.1 equiv). The reaction mixture was purged with vacuum-hydrogen cycles (3×), and stirred at 23° C. under hydrogen. After 5 h, the reaction was heated to 45° C. After 24 h, the reaction was cooled to 23° C., and filtered through celite. The filter cake was washed with tetrahydrofuran (100 mL), the filtrates combined, concentrated in vacuo, and purified by silica gel chromatography (eluant: 0.5-4% methanol/dichloromethane), affording 3-(2-(4-(pyridin-2-ylamino)phenoxy)pyridin-3-yl)cyclopentanol (94 mg, 49% yield). MS (ESI, pos. ion) m/z: 348.1 (M+1). IC50 (uM) 0.010.

1. customThe reaction mixture was purged with vacuum-hydrogen cycles (3×)
2. temperaturethe reaction was heated to 45° C
3. waitAfter 24 h
4. temperaturethe reaction was cooled to 23° C.
5. filtrationfiltered through celite
6. washThe filter cake was washed with tetrahydrofuran (100 mL)
7. concentrationconcentrated in vacuo
8. custompurified by silica gel chromatography (eluant: 0.5-4% methanol/dichloromethane)