反应详情

2.0 g (60%, 51 mmol) of sodium hydride was suspended in 10 ml of N,N-dimethylformamide, and 11.3 g (51 mmol) of ethyl diethylphosphonoacetate was dropped into the suspension under cooling with ice. The obtained mixture was stirred at room temperature for one hour, followed by the addition of 5.5 g (25 mmol) of 1-[1-(1-methylethyl)-1,2,3,4-tetra-hydroquinolin-6-yl]ethanone. The obtained mixture was stirred at 60° C. for 48 hours, followed by the addition of water. The mixture thus obtained was extracted with ethyl acetate. The organic phase was washed with a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate and concentrated in a vacuum. The residue was purified by silica gel column chromatography (4% ethyl acetate/n-hexane) to give 4.0 g of the title compound as a colorless oil.

1. temperatureunder cooling with ice
2. stirringThe obtained mixture was stirred at 60° C. for 48 hours
3. customThe mixture thus obtained
4. extractionwas extracted with ethyl acetate
5. washThe organic phase was washed with a saturated aqueous solution of common salt
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated in a vacuum
8. customThe residue was purified by silica gel column chromatography (4% ethyl acetate/n-hexane)