反应详情

温度

100 °C

2-Bromo-1-(4-hydroxyphenyl)ethanone (2.90 g) and 2-(4-chlorophenoxy)acetamide (5.0 g) were added to N-methylpyrrolidone (5 ml), and the mixture was stirred at 100° C. under a nitrogen atmosphere. After being cooled to room temperature, ethyl acetate and a saturated sodium hydrogen carbonate aqueous solution were added to the reaction mixture and separated into layers. The organic layer was washed with water, dried over sodium sulfate, and then concentrated under reduced pressure. Sodium acetate (11.1 g) in DMF (20 ml) were added to the residue and then stirred at room temperature for 2 hours. The reaction mixture was diluted with ethyl acetate and the prepared insoluble matter was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1) and recrystallized from hexane-ethyl acetate to afford the title compound as a pale yellow powder (1.63 g).

1. temperatureAfter being cooled to room temperature
2. customseparated into layers
3. washThe organic layer was washed with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. additionSodium acetate (11.1 g) in DMF (20 ml) were added to the residue
7. stirringstirred at room temperature for 2 hours
8. additionThe reaction mixture was diluted with ethyl acetate
9. customthe prepared insoluble matter was removed by filtration
10. concentrationthe filtrate was concentrated under reduced pressure
11. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1)
12. customrecrystallized from hexane-ethyl acetate