反应详情

温度

70 °C

To a solution of 0.34 g (15.1 mmol) of sodium in 8 mL of anhydrous MeOH are added dropwise, at room temperature and under argon, 1.6 mL (15.1 mmol) of methyl acetoacetate. After stirring for 30 minutes, 3.25 g (15.11 mmol) of 1-(bromomethyl)-3-(methoxymethyl)benzene are rapidly added dropwise and the reaction medium is then heated for 2 hours 30 minutes at 70° C. The reaction medium is then concentrated under reduced pressure, and the residue obtained is purified by chromatography on a column of silica gel, eluting with a cyclohexane/EtOAc gradient of 0 to 20% EtOAc. 3.2 g of methyl 2-[3-(methoxymethyl)benzyl]-3-oxobutanoate are obtained in the form of an oil.

1. concentrationThe reaction medium is then concentrated under reduced pressure
2. customthe residue obtained
3. customis purified by chromatography on a column of silica gel
4. washeluting with a cyclohexane/EtOAc gradient of 0 to 20% EtOAc