反应详情

温度

80 °C

To Fe powder (61.3 mg, 1.09 mmol), AcOH (2 mL) was added dropwise and heated to 80° C. To it, a solution of 4-chloro-N-[2-(2-chloro-5-nitro-benzoyl)-5-methyl-pyridin-3-yl]-3-trifluoromethyl-benzenesulfonamide (136 mg, 0.255 mmol) in AcOH (2 mL) was added slowly. After 30 min, reaction mixture was allowed to cool to room temperature and diluted with EtOAc (25 mL), filtered through a pad of Celite. The filter cake was washed with EtOAc (25 mL) and the filtrate was concentrated. The residual liquid was slowly treated with saturated aqueous NaHCO3 solution, followed by small portions of solid NaHCO3 to neutralize the AcOH, extracted with EtOAc (2×25 mL) and the extracts were dried (anhydrous Na2SO4), concentrated under reduced pressure and purified (SiO2, EtOAc) to get N-[2-(5-amino-2-chloro-benzoyl)-5-methyl-pyridin-3-yl]-4-chloro-3-trifluoromethyl-benzenesulfonamide (118 mg) in 92.2% yield. ESMS m/z (relative intensity): 504 (M+H)+ (100).

1. customreaction mixture
2. temperatureto cool to room temperature
3. filtrationfiltered through a pad of Celite
4. washThe filter cake was washed with EtOAc (25 mL)
5. concentrationthe filtrate was concentrated
6. additionThe residual liquid was slowly treated with saturated aqueous NaHCO3 solution
7. extractionextracted with EtOAc (2×25 mL)
8. dry with materialthe extracts were dried (anhydrous Na2SO4)
9. concentrationconcentrated under reduced pressure
10. custompurified (SiO2, EtOAc)