反应详情

温度

70 °C

To a suspension of 4-[1-ethyl-3-(4-nitrophenyl)-1H-pyrazol-4-yl]-5-fluoro-1H-pyrrolo[2,3-b]pyridine (0.655 mmol) in ethanol (3.5 mL) was added tin(0) powder (3.28 mmol) and 6N aqueous hydrochloric acid (3.5 mL) and the mixture was heated to 70° C. for 1 h. The reaction mixture was allowed to cool to room temperature, filtered through a pad of celite. The filtrate was diluted with ethyl acetate (10 mL) and washed with 1N sodium hydroxide (5 m L). The aqueous layer was extracted with ethyl acetate (3×10 mL) and the combined extracts were dried over sodium sulfate, filtered through a pad of celite and concentrated under reduced pressure to give the title compound as a yellow solid which was used without further purification. ESMS [M+H]+: 322

1. temperatureto cool to room temperature
2. filtrationfiltered through a pad of celite
3. additionThe filtrate was diluted with ethyl acetate (10 mL)
4. washwashed with 1N sodium hydroxide (5 m L)
5. extractionThe aqueous layer was extracted with ethyl acetate (3×10 mL)
6. dry with materialthe combined extracts were dried over sodium sulfate
7. filtrationfiltered through a pad of celite
8. concentrationconcentrated under reduced pressure