反应详情

11.2 g of 60% oily sodium hydride was suspended in 200 ml of dimethylformamide, and a solution of 56.0 g of 4-phenoxyphenylacetone in 100 ml of dimethylformamide, was added under cooling with ice with stirring, followed by stirring at the same temperature for 5 minutes and at room temperature for 30 minutes. Then, the reaction solution was again cooled with ice, and 52.0 g of phenethyl bromide was added. The reaction solution was gradually returned to room temperature and then stirred for 30 minutes, and water was added to the reaction solution, followed by extraction with ethyl ether. The organic layer was washed with a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate. The drying agent was filtered off, and then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1) to obtain 50.6 g (yield: 61%) of the above identified compound as a pale yellow oily substance.

1. temperatureunder cooling with ice
2. stirringby stirring at the same temperature for 5 minutes and at room temperature for 30 minutes
3. additionwas added
4. customwas gradually returned to room temperature
5. stirringstirred for 30 minutes
6. extractionfollowed by extraction with ethyl ether
7. washThe organic layer was washed with a saturated sodium chloride aqueous solution
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationThe drying agent was filtered off
10. distillationthe solvent was distilled off under reduced pressure
11. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1)
12. customto obtain 50.6 g (yield: 61%) of the