反应详情

温度

0 °C

Isopropylmagnesium chloride (5 mL, 10 mmol, 2 M in diethyl ether) was placed in a dry flask and cooled to 0° C. 3-Ethoxycyclopentenone (0.88 g, 7 mmol) was added dropwise to the solution of the Grignard reagent, and the resulting mixture was stirred at room temperature for 23 h. At this point, 1 M HCl (15 mL) was added gradually, the aqueous phase was separated and extracted 3×with diethyl ether. The combined organic phases were dried over MgSO4, filtered, and concentrated in vacuo. The product was purified first by Kugelrohr distillation (0.1 torr, 120° C.), then by flash chromatography (1:1 pentane:ether) to afford the product as a colorless liquid (0.171 g, 20%). Spectroscopic data were consistent with previously reported data for this compound.7

1. customthe aqueous phase was separated
2. extractionextracted 3×with diethyl ether
3. dry with materialThe combined organic phases were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. distillationThe product was purified first by Kugelrohr distillation (0.1 torr, 120° C.)