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 mL). 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 mL)
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