反应详情

Diethyl 2-(2-(3-chlorophenyl)-2-methylpropanoyl)malonate (8.76 g, 26 mmol) was added to H2SO4 (60 mL, 710 mmol), and the mixture was stirred at room temperature for 45 minutes. Ice (H2O) was added, and the aqueous mixture was extracted with EtOAc (2×). The combined organic layers were washed with water (2×) and brine, dried (MgSO4), and concentrated in vacuo to give the crude compound as an orange oil. The crude oil was purified by silica flash chromatography (0-50% DCM/hexane) to give the desired compound as a white solid (3.90 g). MS (m/e)=295.1 (M+H)+.

1. additionIce (H2O) was added
2. extractionthe aqueous mixture was extracted with EtOAc (2×)
3. washThe combined organic layers were washed with water (2×) and brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customto give the crude compound as an orange oil
7. customThe crude oil was purified by silica flash chromatography (0-50% DCM/hexane)