反应详情

4-Fluoro-N-{[1-(4-methoxybenzyl)-2-oxo-6-(2-oxopyrrolidin-1-yl)-4-(trifluoromethyl)-1,4-dihydro-2H-3,1-benzoxazin-4-yl]methyl}benzamide (30 mg, 0.0525 mmol), aluminum trichloride (70 mg, 0.525 mmol) were mixed in anisole (0.5 mL), and the mixture was stirred at room temperature. After all the ingredients were dissolved, the temperature of the solution was raised to 100° C. and the solution was stirred for 4 hours. The temperature of the solution was brought to room temperature and the solution was diluted with ethyl acetate and then water was added thereto. Then, the organic layer was separated and washed with saturated brine and then dried over magnesium sulfate. After the drying agent was removed by filtration, the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/0), and a crude product was crystallized from ethyl acetate-diisopropyl ether, whereby the objective compound (10.1 mg, 43%) was obtained as a pale yellow solid.

1. dissolutionAfter all the ingredients were dissolved
2. temperaturethe temperature of the solution was raised to 100° C.
3. stirringthe solution was stirred for 4 hours
4. customwas brought to room temperature
5. customThen, the organic layer was separated
6. washwashed with saturated brine
7. dry with materialdried over magnesium sulfate
8. customAfter the drying agent was removed by filtration
9. customthe solvent was evaporated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/0)
11. customa crude product was crystallized from ethyl acetate-diisopropyl ether, whereby the objective compound (10.1 mg, 43%)
12. customwas obtained as a pale yellow solid