反応 #46161

反応方程式

sodium hydride

1-(3-Benzyloxyphenyl)ethanone

diethyl carbonate

acetic acid

→

3-(3-benzyloxyphenyl)-3-oxopropionate ethyl ester

収率 84.0%

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate/saturated sodium chloride
2. 2
   その他the organic layer was separated
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   その他The solvent was removed under a reduced pressure
5. 5
   その他the resulting residue was purified by column chromatography (ethyl acetate:hexane=1:10)

実験手順

1-(3-Benzyloxyphenyl)ethanone (218 g, 966.10 mmol) was dissolved in diethyl carbonate and sodium hydride (60% oil) (46.37 g, 1.15 mmol) was slowly added thereto at 0° C., and then stirred for 3 hours at 60° C. After the reaction was completed, ice water and acetic acid were added to the reaction mixture, extracted with ethyl acetate/saturated sodium chloride, the organic layer was separated, and dried over anhydrous magnesium sulfate. The solvent was removed under a reduced pressure and the resulting residue was purified by column chromatography (ethyl acetate:hexane=1:10) to obtain 3-(3-benzyloxyphenyl)-3-oxopropionate ethyl ester (184.68 g, yield 84%) in an oil state.

出典