反应详情

To a solution of dimethyl malonate (4.96 mL, 43 mmol) in DMF (80 mL) was added NaH (1.3 g 80% in mineral oil). After 20 min. a solution of 1-(bromomethyl)-4-(diethoxymethyl)benzene (2.37 g, 8.7 mmol) in DMF (5 mL) was added via double-tipped needle. After 1 h at 0° C., the reaction was quenched by the addition of saturated NH4Cl solution. The product was extracted with Et2O and the organic layer wash washed with H2O and brine. After drying (MgSO4) and filtration, the solvent was removed under vacuum. The crude was purified by flash chromatography (1:10 EtOAc/hexane) to yield a colorless oil (1:42 g).

1. customthe reaction was quenched by the addition of saturated NH4Cl solution
2. extractionThe product was extracted with Et2O
3. washthe organic layer wash
4. washwashed with H2O and brine
5. customAfter drying
6. filtration(MgSO4) and filtration
7. customthe solvent was removed under vacuum
8. customThe crude was purified by flash chromatography (1:10 EtOAc/hexane)
9. customto yield a colorless oil (1:42 g)