反应详情

To a solution of tert-butyl {3-[(2-amino[1,2,4]triazolo[1,5-a]pyridin-6-yl)oxy]phenyl}carbamate (10.5 g, 30.8 mmol) in N,N-dimethylacetamide (40 mL) was added with stirring under ice-cooling cyclopropanecarbonyl chloride (8.39 mL, 92.4 mmol), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, trifluoroacetic acid (50 mL) was added to the residue, and the mixture was stirred at 0° C. for 30 min. The solvent was evaporated under reduced pressure, and the residue was dissolved in water. The mixture was neutralized with saturated aqueous sodium hydrogen carbonate solution and extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, and the residue was collected by filtration and washed with ethyl acetate-hexane to give the title compound (7.44 g, 78%) as a white solid.

1. stirringthe mixture was stirred at room temperature for 2 hr
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltrated
6. concentrationThe filtrate was concentrated under reduced pressure, trifluoroacetic acid (50 mL)
7. additionwas added to the residue
8. stirringthe mixture was stirred at 0° C. for 30 min
9. customThe solvent was evaporated under reduced pressure
10. dissolutionthe residue was dissolved in water
11. extractionextracted with ethyl acetate
12. washThe organic layer was washed with water and saturated brine
13. dry with materialdried over anhydrous magnesium sulfate
14. filtrationfiltrated
15. concentrationThe filtrate was concentrated under reduced pressure
16. filtrationthe residue was collected by filtration
17. washwashed with ethyl acetate-hexane