反应详情

温度

110 °C

To a solution of N-{[6-bromo-1-(4-methoxybenzyl)-2-oxo-4-(trifluoromethyl)-1,4-dihydro-2H-3,1-benzoxazin-4-yl]methyl}-4-fluorobenzamide (1.18 g, 2.08 mmol), copper iodide (I) (79 mg, 0.416 mmol) and sodium iodide (624 mg, 4.16 mmol) in dioxane (4.2 mL), N,N′-dimethylethylene diamine (89 μL, 0.832 mmol) was added at room temperature. The reaction solution was stirred for 5 hours under heating at 110° C. The temperature of the solution was brought to room temperature, and the solution was diluted with ethyl acetate, which was washed sequentially with a saturated aqueous ammonium chloride solution and saturated brine and then dried over magnesium sulfate. After the drying agent was removed by filtration, the solvent was evaporated under reduced pressure. The resulting solid was washed with hexane and ethyl acetate, whereby the objective compound (995 mg, 78%) was obtained as a white solid.

1. customwas brought to room temperature
2. washwas washed sequentially with a saturated aqueous ammonium chloride solution and saturated brine
3. dry with materialdried over magnesium sulfate
4. customAfter the drying agent was removed by filtration
5. customthe solvent was evaporated under reduced pressure
6. washThe resulting solid was washed with hexane and ethyl acetate, whereby the objective compound (995 mg, 78%)
7. customwas obtained as a white solid