反应详情

A mixed solution of 2-chloro-3-(1-cyanocyclopropyl)-N-{2,4-difluoro-5-[(5-nitropyridin-2-yl)oxy]phenyl}benzamide (5.20 g, 11 mmol), iron powder (1.24 g, 22 mmol) and calcium chloride (2.45 g, 22 mmol) in ethanol (80 mL)-water (20 mL) was stirred at 80° C. overnight. The reaction mixture was poured into 0.5N aqueous sodium hydroxide solution (500 mL), ethyl acetate (300 mL) was added, the mixture was stirred, and the insoluble material was filtered through celite. The ethyl acetate layer was separated from the filtrate, and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was triturated with diethyl ether to give the title compound (4.25 g, 88%) as a pale-yellow amorphous.

1. additionwas added
2. filtrationthe insoluble material was filtered through celite
3. customThe ethyl acetate layer was separated from the filtrate
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationThe insoluble material was filtered off
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe obtained residue was triturated with diethyl ether