反应详情

Jones' reagent (75 ml of 1.67 M solution, 125 mmol) is added dropwise over 30 minutes to a cooled (ice-bath) solution of 5-(5-bromo-4-ethylphenyl)-4-hydroxycyclopent-2-enone (33 g, 117 mmol) in acetone (400 ml). The mixture is stirred for 20 minutes, then the cooling bath is removed and the mixture is stirred for 1 hour at room temperature. Isopropanol (150 ml) is added to the yellow slurry and the mixture is stirred at room temperature for 2 hours. The mixture is diluted with ethyl acetate and washed with brine, dried over anhydrous magnesium sulfate, filtered and the filtrate is evaporated under reduced pressure to give 2-(5-bromo-2-ethylphenyl)cyclopent-4-ene-1,3-dione.

1. customthe cooling bath is removed
2. stirringthe mixture is stirred for 1 hour at room temperature
3. additionIsopropanol (150 ml) is added to the yellow slurry
4. stirringthe mixture is stirred at room temperature for 2 hours
5. additionThe mixture is diluted with ethyl acetate
6. washwashed with brine
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. customthe filtrate is evaporated under reduced pressure