反应详情

To a solution of 5-(3-aminophenoxy)pyridine-2-amine dihydrochloride (3.5 g, 12.7 mmol) in N,N-dimethylacetamide (30 mL) was added 3-(trifluoromethyl)benzoylchloride (2.80 g, 13.4 mmol), and the mixture was stirred at room temperature for 6 hr. The reaction mixture was concentrated under reduced pressure, 5% aqueous sodium hydrogen carbonate solution (100 mL) was added to the residue, and the mixture was extracted with ethyl acetate (200 mL). The organic layer was washed with water (100 mL) and saturated brine (100 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. Ethyl acetate (30 mL)/hexane (20 mL) was added to the obtained residue, and the obtained precipitate was collected by filtration and air-dried to give the title compound (3.95 g, 83%) as a colorless powder.

1. concentrationThe reaction mixture was concentrated under reduced pressure, 5% aqueous sodium hydrogen carbonate solution (100 mL)
2. additionwas added to the residue
3. extractionthe mixture was extracted with ethyl acetate (200 mL)
4. washThe organic layer was washed with water (100 mL) and saturated brine (100 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationThe insoluble material was filtered off
7. concentrationthe filtrate was concentrated under reduced pressure
8. additionEthyl acetate (30 mL)/hexane (20 mL) was added to the obtained residue
9. filtrationthe obtained precipitate was collected by filtration
10. customair-dried