反应详情

To a solution of diethyl 2-phenylmalonate (100 mmol) in anhydrous tetrahydrofuran (300 mL) is added sodium ethoxide (110 mmol). The mixture is stirred at room temperature for 30 min, followed by the addition of a solution of acetyl chloride (110 mmol) in tetrahydrofuran (50 mL). After the addition is complete, the mixture is heated to reflux for 3 hours, cooled to room temperature, neutralized with 2 N HCl, then concentrated in vacuo. The residue is partitioned between H20 and CHCl3, the organic extracts washed with sodium bicarbonate, water, and brine, dried (MgS04), filtered and concentrated.

1. additionAfter the addition
2. temperaturethe mixture is heated
3. temperatureto reflux for 3 hours
4. temperaturecooled to room temperature
5. concentrationconcentrated in vacuo
6. customThe residue is partitioned between H20 and CHCl3
7. washthe organic extracts washed with sodium bicarbonate, water, and brine
8. customdried (MgS04)
9. filtrationfiltered
10. concentrationconcentrated