反应详情

温度

70 °C

To a solution of 4-[1-ethyl-3-(4-nitrophenyl)-1H-pyrazol-4-yl]-1-(phenylsulfonyl)-2-[4-(1-pyrrolidinylmethyl)phenyl]-1H-pyrrolo[2,3-b]pyridine (0.487 mmol) in glacial acetic acid (4 mL) was added zinc powder (3.41 mmol). After 1 h, the reaction was filtered and the zinc residue was rinsed with acetic acid. The filtrate was concentrated under reduced pressure and azeotroped five times with 1:1 methanol/toluene to remove residual acetic acid. The crude aniline was dissolved in methanol, treated with 6N NaOH (1.46 mmol) and heated to 70° C. After 5 h, the reaction mixture was concentrated under reduced pressure and the residue was suspended in cold water and stirred vigorously. The precipitate was collected by filtration and dried to constant weight under high vacuum to give title compound. ESMS [M+H]+: 463.4

1. filtrationthe reaction was filtered
2. washthe zinc residue was rinsed with acetic acid
3. concentrationThe filtrate was concentrated under reduced pressure
4. customazeotroped five times with 1:1 methanol/toluene
5. customto remove residual acetic acid
6. dissolutionThe crude aniline was dissolved in methanol
7. waitAfter 5 h
8. concentrationthe reaction mixture was concentrated under reduced pressure
9. filtrationThe precipitate was collected by filtration
10. customdried to constant weight under high vacuum