反应详情

1.49 g of triethylamine was gradually dropwise added to a mixed solution comprising 0.8 g of cyclopropylmethylamine hydrochloride and 40 ml of tetrahydrofuran under cooling with ice, followed by stirring at room temperature for 30 minutes. Then, a mixed solution comprising 1 g of 2-[1-(3-chloro-2-pyridyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl]-8-methyl-4H-3,1-benzoxazin-4-one and 10 ml of tetrahydrofuran was gradually dropwise added. After completion of the dropwise addition, the mixed solution was reacted for 4 hours under reflux. After completion of the reaction, the solvent was distilled off under reduced pressure, and to the residue, ethyl acetate and water were added for extraction. The organic layer was washed with water and a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1) to obtain 0.54 g of the desired product having a melting point of 199.4° C.

1. temperatureunder cooling with ice
2. additionwas gradually dropwise added
3. additionAfter completion of the dropwise addition
4. customthe mixed solution was reacted for 4 hours
5. temperatureunder reflux
6. customAfter completion of the reaction
7. distillationthe solvent was distilled off under reduced pressure
8. additionto the residue, ethyl acetate and water were added for extraction
9. washThe organic layer was washed with water
10. dry with materiala saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate
11. distillationThe solvent was distilled off under reduced pressure
12. customthe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1)